An exceptional 5:4 enantiomeric structure
Wachter, Erin; Glazer, Edith C.; Parkin, Sean; Brock, Carolyn Pratt; Acta Crystallographica Section B 72 (2016) 223–231; doi:10.1107/S205252061600127X

data_2107483
_publ_section_title
;
 An exceptional 5:4 enantiomeric structure
;
_journal_coeditor_code           BM5083
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              223
_journal_page_last               231
_journal_paper_doi               10.1107/S205252061600127X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_moiety
'(C42 H32 N8 Ru), 2(F6 P), 0.111 (C4 H10 O), 1.222(C3 H6 O)'
_chemical_formula_sum            'C46.111 H40.444 F12 N8 O1.333 P2 Ru'
_chemical_formula_weight         1118.98
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014/7 and CIFFIX'
_cell_angle_alpha                81.8740(10)
_cell_angle_beta                 89.2110(10)
_cell_angle_gamma                69.1080(10)
_cell_formula_units_Z            9
_cell_length_a                   18.3127(3)
_cell_length_b                   21.3286(4)
_cell_length_c                   29.2640(6)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.15
_cell_measurement_theta_min      2.75
_cell_volume                     10563.1(3)
_computing_cell_refinement       '<i>APEX2</i> (Bruker-AXS, 2006)'
_computing_data_collection       '<i>APEX2</i> (Bruker-AXS, 2006)'
_computing_data_reduction        '<i>APEX2</i> (Bruker-AXS, 2006)'
_computing_molecular_graphics    '<i>XP in SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELX</i> (Sheldrick, 2008) and <i>CIFFIX</i> (Parkin, 2013)'
_computing_structure_refinement  '<i>SHELXL-2014/7</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker X8 Proteum diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            139158
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.284
_diffrn_reflns_theta_min         2.241
_exptl_absorpt_coefficient_mu    4.192
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Krause et al., 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       'small cut block'
_exptl_crystal_F_000             5092
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.997
_refine_diff_density_min         -1.296
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.188(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5769
_refine_ls_number_reflns         41744
_refine_ls_number_restraints     6050
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+31.8949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                38577
_reflns_number_total             41744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bm5083sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C46.111 H40.444 F12 N8 O1.333 P2 Ru1'
_cod_database_code               2107483
_shelx_estimated_absorpt_t_min   0.656
_shelx_estimated_absorpt_t_max   0.818
_shelx_hkl_checksum              2807
_shelx_res_checksum              39098
_shelx_fab_checksum              8423
_cod_database_fobs_code 2107483