Detailed example of the identification and crystallographic analysis of a pseudo-merohedrally twinned crystal
Guzei, Ilia; Herbst-Irmer, Regine; Munyaneza, Apollinaire; Darkwa, James; Acta Crystallographica Section B 68 (2012) 150–157; doi:10.1107/S0108768112002728

data_2105087
_publ_section_title
;
 Detailed example of the identification and crystallographic analysis of a
 pseudo-merohedrally twinned crystal
;
_journal_coeditor_code           PS5014
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              150
_journal_page_last               157
_journal_paper_doi               10.1107/S0108768112002728
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C44 H42 Br5 Fe3 N6 Ni O4'
_chemical_formula_sum            'C44 H42 Br5 Fe3 N6 Ni O4'
_chemical_formula_weight         1344.65
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 118.393(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2181(3)
_cell_length_b                   22.0080(3)
_cell_length_c                   16.0005(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.05
_cell_measurement_theta_min      3.14
_cell_volume                     4714.25(17)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.50\% \w and 0.5 \% \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35920
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         72.05
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    13.067
_exptl_absorpt_correction_T_max  0.3762
_exptl_absorpt_correction_T_min  0.1860
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2644
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.659
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8033
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                7903
_reflns_number_total             8033
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ps5014.cif
_cod_data_source_block           I
_cod_original_cell_volume        4714.25(14)
_cod_original_sg_symbol_Hall     'C -2yc      '
_cod_original_sg_symbol_H-M      'C 1 c 1     '
_cod_database_code               2105087