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quinacridone-beta.cif
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quinacridone-beta.cif
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# Attachment 'beta_chin.CIF'
data_0231
_database_code_depnum_ccdc_archive 'CCDC 620258'
_audit_creation_method 'SHELXTL-plus (Sheldrick, 1997)'
_chemical_name_systematic
;
7,14-dioxo-5,7,12,14-tetrahydro-chinolino-[2,3-b]-acridin
;
_chemical_name_common
'beta-quinacridone (Pigment Violet 19, beta phase)'
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C20 H12 N2 O2'
_chemical_formula_weight 312.32
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'
_cell_length_a 5.692(1)
_cell_length_b 3.975(1)
_cell_length_c 30.02(4)
_cell_angle_alpha 90.00
_cell_angle_beta 96.76(6)
_cell_angle_gamma 90.00
_cell_volume 674.5(9)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 18
_cell_measurement_theta_min 3.5
_cell_measurement_theta_max 11
_exptl_crystal_description 'very thin crystals'
_exptl_crystal_colour red-violet
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas 1.54
_exptl_crystal_density_diffrn 1.538
_exptl_crystal_density_method
;
suspension in aqueous K(2)HgJ(4)-solution
;
_exptl_crystal_F_000 324
_exptl_absorpt_coefficient_mu 0.101
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_special_details
;
The crystal was fixed in a Mark tube by a tiny bit of grease.
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71070
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
;
computer controlled 4-circle diffractometer P3 (Nicolet)
with a scintillation counter
;
_diffrn_measurement_method 'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 1
_diffrn_standards_interval_count '68 reflections'
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% 'no decay'
_diffrn_reflns_number 2124
_diffrn_reflns_av_R_equivalents 0.1302
_diffrn_reflns_av_sigmaI/netI 0.1753
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_theta_min 2.73
_diffrn_reflns_theta_max 24.00
_reflns_number_total 1064
_reflns_number_gt 363
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Nicolet software'
_computing_cell_refinement 'Nicolet software'
_computing_data_reduction 'Nicolet software'
_computing_structure_solution 'SHELXTL-plus (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXTL-plus (Sheldrick, 1997)'
_computing_molecular_graphics 'SHELXTL-plus (Sheldrick, 1997)'
_computing_publication_material 'SHELXTL-plus (Sheldrick, 1997)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1064
_refine_ls_number_parameters 109
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1997
_refine_ls_R_factor_gt 0.0898
_refine_ls_wR_factor_ref 0.2728
_refine_ls_wR_factor_gt 0.2057
_refine_ls_goodness_of_fit_ref 0.908
_refine_ls_restrained_S_all 0.908
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.2030(8) 0.4159(15) 0.08727(15) 0.0593(17) Uani 1 1 d . . .
N1 N 0.7900(9) -0.1576(17) 0.07783(18) 0.0466(18) Uani 1 1 d . . .
H1 H 0.9147 -0.2762 0.0758 0.046 Uiso 1 1 calc R . .
C01 C 0.4916(13) 0.221(2) 0.1677(2) 0.057(2) Uani 1 1 d . . .
H01 H 0.3580 0.3469 0.1717 0.059 Uiso 1 1 calc R . .
C02 C 0.6420(13) 0.125(2) 0.2043(3) 0.059(2) Uani 1 1 d . . .
H02 H 0.6062 0.1754 0.2330 0.077 Uiso 1 1 calc R . .
C03 C 0.8501(12) -0.050(2) 0.1986(2) 0.056(2) Uani 1 1 d . . .
H03 H 0.9560 -0.1030 0.2236 0.073 Uiso 1 1 calc R . .
C04 C 0.9001(12) -0.143(2) 0.1572(2) 0.053(2) Uani 1 1 d . . .
H04 H 1.0386 -0.2599 0.1539 0.065 Uiso 1 1 calc R . .
C05 C 0.7430(10) -0.062(2) 0.1197(2) 0.046(2) Uani 1 1 d . . .
C06 C 0.5353(11) 0.133(2) 0.1242(2) 0.046(2) Uani 1 1 d . . .
C07 C 0.6497(10) -0.076(2) 0.0385(2) 0.0425(19) Uani 1 1 d . . .
C08 C 0.4406(11) 0.110(2) 0.0414(2) 0.0411(18) Uani 1 1 d . . .
C09 C 0.3805(12) 0.228(2) 0.0847(2) 0.0429(19) Uani 1 1 d . . .
C10 C 0.2955(11) 0.181(2) 0.0021(2) 0.043(2) Uani 1 1 d . . .
H10 H 0.1573 0.3033 0.0036 0.057 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.038(3) 0.084(4) 0.056(3) -0.006(3) 0.009(2) 0.015(3)
N1 0.036(3) 0.056(5) 0.047(4) 0.010(3) 0.001(3) 0.010(3)
C01 0.048(4) 0.083(7) 0.041(4) 0.002(5) 0.011(3) 0.004(5)
C02 0.066(5) 0.063(6) 0.052(5) 0.004(5) 0.018(4) -0.008(5)
C03 0.053(4) 0.052(6) 0.061(5) -0.004(5) 0.001(4) 0.014(5)
C04 0.041(4) 0.064(6) 0.050(4) 0.003(5) -0.007(3) 0.009(4)
C05 0.029(3) 0.076(7) 0.034(4) 0.001(4) 0.003(3) 0.001(4)
C06 0.029(3) 0.064(6) 0.046(4) 0.009(5) 0.001(3) 0.002(4)
C07 0.030(3) 0.047(5) 0.050(4) 0.013(4) 0.002(3) 0.002(4)
C08 0.034(3) 0.051(5) 0.039(4) -0.005(4) 0.006(3) -0.004(4)
C09 0.040(4) 0.043(5) 0.046(4) 0.001(4) 0.007(3) 0.000(4)
C10 0.031(3) 0.052(6) 0.047(4) 0.000(4) 0.009(3) 0.008(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C09 1.265(8) . ?
N1 C05 1.370(8) . ?
N1 C07 1.384(8) . ?
N1 H1 0.8600 . ?
C01 C02 1.365(9) . ?
C01 C06 1.401(9) . ?
C01 H01 0.9300 . ?
C02 C03 1.401(10) . ?
C02 H02 0.9300 . ?
C03 C04 1.359(8) . ?
C03 H03 0.9300 . ?
C04 C05 1.389(8) . ?
C04 H04 0.9300 . ?
C05 C06 1.433(10) . ?
C06 C09 1.442(9) . ?
C07 C10 1.360(9) 3_655 ?
C07 C08 1.413(9) . ?
C08 C10 1.387(9) . ?
C08 C09 1.459(9) . ?
C10 C07 1.360(9) 3_655 ?
C10 H10 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C05 N1 C07 124.2(6) . . ?
C05 N1 H1 117.9 . . ?
C07 N1 H1 117.9 . . ?
C02 C01 C06 121.1(7) . . ?
C02 C01 H01 119.5 . . ?
C06 C01 H01 119.5 . . ?
C01 C02 C03 120.0(7) . . ?
C01 C02 H02 120.0 . . ?
C03 C02 H02 120.0 . . ?
C04 C03 C02 121.2(7) . . ?
C04 C03 H03 119.4 . . ?
C02 C03 H03 119.4 . . ?
C03 C04 C05 119.5(7) . . ?
C03 C04 H04 120.2 . . ?
C05 C04 H04 120.2 . . ?
N1 C05 C04 120.1(7) . . ?
N1 C05 C06 119.3(6) . . ?
C04 C05 C06 120.6(6) . . ?
C01 C06 C05 117.5(6) . . ?
C01 C06 C09 122.8(7) . . ?
C05 C06 C09 119.7(6) . . ?
C10 C07 N1 121.5(7) 3_655 . ?
C10 C07 C08 120.1(6) 3_655 . ?
N1 C07 C08 118.4(6) . . ?
C10 C08 C07 118.3(6) . . ?
C10 C08 C09 120.9(7) . . ?
C07 C08 C09 120.7(6) . . ?
O1 C09 C06 121.3(7) . . ?
O1 C09 C08 121.0(6) . . ?
C06 C09 C08 117.6(7) . . ?
C07 C10 C08 121.6(6) 3_655 . ?
C07 C10 H10 119.2 3_655 . ?
C08 C10 H10 119.2 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C06 C01 C02 C03 3.3(13) . . . . ?
C01 C02 C03 C04 -3.6(13) . . . . ?
C02 C03 C04 C05 0.4(13) . . . . ?
C07 N1 C05 C04 -177.0(8) . . . . ?
C07 N1 C05 C06 0.6(11) . . . . ?
C03 C04 C05 N1 -179.2(8) . . . . ?
C03 C04 C05 C06 3.1(12) . . . . ?
C02 C01 C06 C05 0.2(12) . . . . ?
C02 C01 C06 C09 179.8(8) . . . . ?
N1 C05 C06 C01 178.9(7) . . . . ?
C04 C05 C06 C01 -3.4(12) . . . . ?
N1 C05 C06 C09 -0.7(12) . . . . ?
C04 C05 C06 C09 177.0(7) . . . . ?
C05 N1 C07 C10 -179.4(8) . . . 3_655 ?
C05 N1 C07 C08 -1.9(11) . . . . ?
C10 C07 C08 C10 0.0(12) 3_655 . . . ?
N1 C07 C08 C10 -177.6(7) . . . . ?
C10 C07 C08 C09 -179.3(7) 3_655 . . . ?
N1 C07 C08 C09 3.1(10) . . . . ?
C01 C06 C09 O1 4.4(12) . . . . ?
C05 C06 C09 O1 -176.0(7) . . . . ?
C01 C06 C09 C08 -177.7(7) . . . . ?
C05 C06 C09 C08 1.9(11) . . . . ?
C10 C08 C09 O1 -4.5(11) . . . . ?
C07 C08 C09 O1 174.7(7) . . . . ?
C10 C08 C09 C06 177.6(7) . . . . ?
C07 C08 C09 C06 -3.2(10) . . . . ?
C07 C08 C10 C07 0.0(12) . . . 3_655 ?
C09 C08 C10 C07 179.3(7) . . . 3_655 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O1 0.86 2.04 2.885(8) 165.9 1_645
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 24.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.276
_refine_diff_density_min -0.300
_refine_diff_density_rms 0.077