Oxidation and chalcogenylative disproportionation of anionic phosphide ligands in yttrium complexes with elemental sulfur and selenium.
Zhang, Fangjun; Yi, Weiyin; Zhang, Jie; You, Qing; Weng, Linhong; Zhou, Xigeng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10596–10603; doi:10.1039/c9dt01537j

data_7700220
_publ_section_title
;
 Oxidation and chalcogenylative disproportionation of anionic phosphide
 ligands in yttrium complexes with elemental sulfur and selenium.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10596
_journal_page_last               10603
_journal_paper_doi               10.1039/c9dt01537j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C36 H45 B N6 O2 P S Y'
_chemical_formula_weight         756.53
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-05-22 deposited with the CCDC.    2019-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.461(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.950(6)
_cell_length_b                   13.491(7)
_cell_length_c                   13.080(7)
_cell_measurement_reflns_used    833
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.15
_cell_measurement_theta_min      3.01
_cell_volume                     1862.3(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0710
_diffrn_reflns_av_unetI/netI     0.1288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8111
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.599
_diffrn_reflns_theta_min         1.615
_exptl_absorpt_coefficient_mu    1.705
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
; 
 Flack x determined using 1164 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.033(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6633
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+8.3239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.895
_reflns_Friedel_fraction_max     0.890
_reflns_number_gt                3820
_reflns_number_total             6633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01537j2.cif
_cod_data_source_block           6S
_cod_depositor_comments
'Adding full bibliography for 7700213--7700220.cif.'
_cod_database_code               7700220
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.905
_shelx_res_checksum              85801