Twinning of three Fe-PNP pincer complexes interpreted according to order‒disorder (OD) theory
Bichler, Bernhard; Holzhacker, Christian; Glatz, Mathias; Stöger, Berthold; Kirchner, Karl; Acta Crystallographica Section B 71 (2015) 524–534; doi:10.1107/S2052520615015097

data_2107482
_publ_section_title
;
 Twinning of three Fe-PNP pincer complexes interpreted according to
 order--disorder (OD) theory
;
_journal_coeditor_code           UM5003
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              524
_journal_page_last               534
_journal_paper_doi               10.1107/S2052520615015097
_journal_volume                  71
_journal_year                    2015
_chemical_formula_sum            'C46 H55 Cl2 Fe N3 O5 P2'
_chemical_formula_weight         918.7
_chemical_name_systematic        ' ?'
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_cell_angle_alpha                96.277(3)
_cell_angle_beta                 92.393(3)
_cell_angle_gamma                90.009(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3389(7)
_cell_length_b                   10.3155(8)
_cell_length_c                   24.3224(18)
_cell_measurement_reflns_used    9106
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      2.3
_cell_volume                     2327.0(3)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX 2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_refinement
'JANA20006 (Pet\<r\'i\<cek, M. Du\<sek & L. Palatinus, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.71
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40097
_diffrn_reflns_theta_full        12.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         0.84
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            'translucent yellow'
_exptl_crystal_density_diffrn    1.3107
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.70
_refine_ls_abs_structure_details
'  5587 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.76
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    527
_refine_ls_number_parameters     439
_refine_ls_number_reflns         39775
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.0484
_refine_ls_shift/su_mean         0.0028
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0703
_reflns_number_gt                35102
_reflns_number_total             39775
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            um5003sup1.cif
_cod_data_source_block           Fe_PNP-TADDOL-iPr_Cl2
_cod_original_formula_sum        'C46 H55 Cl2 Fe1 N3 O5 P2'
_cod_database_code               2107482