Crystal structure (7,8-bis(diisopropylphosphino)-7,8-dicarba-nido-undecaborane-κ2 P,P′)-(benzoato-κ2 O,O′)nickel(II), C21H42B9NiO2P2
Liguo, Yang; xin, Wang; Qianqian, Gao; Yuqiang, Dai; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 59–61; doi:10.1515/ncrs-2016-0148

data_8106432
_publ_section_title
;
 Crystal structure
 (7,8-bis(diisopropylphosphino)-7,8-dicarba-nido-undecaborane-\k2
 P,P&#x2032;)-(benzoato-\k2 O,O&#x2032;)nickel(II), C21H42B9NiO2P2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              59
_journal_page_last               61
_journal_paper_doi               10.1515/ncrs-2016-0148
_journal_volume                  232
_journal_year                    2017
_chemical_formula_sum            'C21 H42 B9 Ni O2 P2'
_chemical_formula_weight         544.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 112.250(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3840(9)
_cell_length_b                   17.0119(18)
_cell_length_c                   19.9631(19)
_cell_measurement_reflns_used    2898
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.0085
_cell_measurement_theta_min      2.488
_cell_volume                     2949.6(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14827
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.627
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.8402
_exptl_absorpt_correction_T_min  0.7444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5075
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.4168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2835
_reflns_number_total             5075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2016-0148_suppl.cif
_cod_data_source_block           f
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8106432
_shelx_estimated_absorpt_t_min   0.744
_shelx_estimated_absorpt_t_max   0.840
_shelx_res_checksum              44726
_shelx_hkl_checksum              5587