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_7715491
_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         'C84 H84 B Ba F15 N3 O2 P [+ C6 H14]'
_chemical_formula_sum            'C90 H98 B Ba F15 N3 O2 P'
_chemical_formula_weight         1717.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                80.945(4)
_cell_angle_beta                 67.840(4)
_cell_angle_gamma                88.782(4)
_cell_formula_units_Z            2
_cell_length_a                   15.537(2)
_cell_length_b                   16.193(2)
_cell_length_c                   18.240(2)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.2938
_cell_measurement_theta_min      2.1931
_cell_measurement_wavelength     0.710730
_cell_volume                     4193.4(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 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_orient_matrix_UB_11      -0.0676498
_diffrn_orient_matrix_UB_12      0.0107477
_diffrn_orient_matrix_UB_13      0.0254178
_diffrn_orient_matrix_UB_21      -0.0078564
_diffrn_orient_matrix_UB_22      -0.0495160
_diffrn_orient_matrix_UB_23      0.0426885
_diffrn_orient_matrix_UB_31      0.0141360
_diffrn_orient_matrix_UB_32      0.0367457
_diffrn_orient_matrix_UB_33      0.0336083
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59379
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.625
_diffrn_reflns_theta_min         1.866
_diffrn_source_current           1.0
_diffrn_source_power             50.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.805
_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    1.361
_exptl_crystal_description       prism
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1008
_refine_ls_number_reflns         19189
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+1.6242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                14909
_reflns_number_total             19189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt00487f2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7715491--7715494.cif.'
_cod_database_code               7715491
_shelx_res_checksum              72101
_shelx_fab_checksum              31227