Barium phosphidoboranes and related calcium complexes.
Duneş, Gabriel; Chapple, Peter M.; Kahlal, Samia; Roisnel, Thierry; Carpentier, Jean-François; Saillard, Jean-Yves; Sarazin, Yann; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6892–6905; doi:10.1039/d4dt00487f

data_7715494
_publ_section_title
;
 Barium phosphidoboranes and related calcium complexes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6892
_journal_page_last               6905
_journal_paper_doi               10.1039/d4dt00487f
_journal_volume                  53
_journal_year                    2024
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C70 H40 B2 Ba F30 O2 P2, C7 H8'
_chemical_formula_sum            'C77 H48 B2 Ba F30 O2 P2'
_chemical_formula_weight         1796.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   49.3823(17)
_cell_length_b                   14.4529(5)
_cell_length_c                   21.5081(8)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.1084
_cell_measurement_theta_min      2.3321
_cell_measurement_wavelength     0.710730
_cell_volume                     14630.7(9)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2024)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_orient_matrix_UB_11      0.0054089
_diffrn_orient_matrix_UB_12      0.0529972
_diffrn_orient_matrix_UB_13      -0.0236880
_diffrn_orient_matrix_UB_21      -0.0200143
_diffrn_orient_matrix_UB_22      0.0040371
_diffrn_orient_matrix_UB_23      -0.0292758
_diffrn_orient_matrix_UB_31      -0.0046471
_diffrn_orient_matrix_UB_32      0.0442974
_diffrn_orient_matrix_UB_33      0.0310083
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43203
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         2.205
_diffrn_source_current           1.0
_diffrn_source_power             50.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       prism
_exptl_crystal_F_000             7136
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.230
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         16431
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+1.7129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                12168
_reflns_number_total             16431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt00487f2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7715491--7715494.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7715494
_shelx_res_checksum              6432