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_7715492
_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_absolute_configuration rm/ad/rmad/syn/unk/.
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C62 H82 B2 Ca N3 O P'
_chemical_formula_sum            'C62 H82 B2 Ca N3 O P'
_chemical_formula_weight         977.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_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                 99.281(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0239(10)
_cell_length_b                   12.5202(9)
_cell_length_c                   18.2775(12)
_cell_measurement_reflns_used    7029
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      27.4174
_cell_measurement_theta_min      2.2708
_cell_measurement_wavelength     0.710730
_cell_volume                     2941.3(4)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material
'CRYSCALC (T. Roisnel, local program, ver. 2024)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      299(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_orient_matrix_UB_11      0.0154523
_diffrn_orient_matrix_UB_12      -0.0446245
_diffrn_orient_matrix_UB_13      0.0458316
_diffrn_orient_matrix_UB_21      0.0761698
_diffrn_orient_matrix_UB_22      0.0120485
_diffrn_orient_matrix_UB_23      0.0012680
_diffrn_orient_matrix_UB_31      -0.0035030
_diffrn_orient_matrix_UB_32      0.0651371
_diffrn_orient_matrix_UB_33      0.0311641
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15470
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_min         2.271
_diffrn_source_current           30.
_diffrn_source_power             1500.0
_diffrn_source_voltage           50.
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
Flack x determined using 2986 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         10613
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.7797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.509
_reflns_Friedel_fraction_full    0.614
_reflns_Friedel_fraction_max     0.555
_reflns_number_gt                9566
_reflns_number_total             10613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt00487f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7715491--7715494.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7715492
_shelx_res_checksum              60904