B-substituted group 1 phosphides: Synthesis and reactivity
Aman, Michal; Dostál, Libor; R°užička, Aleš; Ruzickova, Zdenka; Jambor, Roman; Dalton Transactions  (2023) –; doi:10.1039/D3DT02568C

data_7714296
_publ_section_title
;
 B-substituted group 1 phosphides: Synthesis and reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02568C
_journal_year                    2023
_chemical_formula_moiety         'C40 H57 B Na O3 P'
_chemical_formula_sum            'C40 H57 B Na O3 P'
_chemical_formula_weight         650.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'APEX3 v2016.5-0'
_audit_update_record
;
2023-06-06 deposited with the CCDC.	2023-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0350(18)
_cell_length_b                   10.8962(10)
_cell_length_c                   19.662(4)
_cell_measurement_reflns_used    36523
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     3863.8(9)
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34880
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         2.417
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.374
_exptl_crystal_size_min          0.290
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2321 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         8653
_refine_ls_number_restraints     534
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+1.5006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1652
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                6656
_reflns_number_total             8653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02568c7.cif
_cod_data_source_block           5
_cod_original_cell_volume        3863.9(9)
_cod_database_code               7714296
_shelx_shelxl_version_number     2019/1
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.895
;
_shelx_res_checksum              71874