Ligand Attachment Chemistry in the Preparation of PCsp3P and PCsp2P Complexes of Rhodium
Logan, Jessamyn R.; Piers, Warren E.; Borau-Garcia, Javier; Spasyuk, Denis M.; Organometallics 35 (2016) 1279–; doi:10.1021/acs.organomet.6b00155

data_4088529
_publ_section_title
;
 Ligand Attachment Chemistry in the Preparation of PCsp3P and PCsp2P
 Complexes of Rhodium
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1279
_journal_paper_doi               10.1021/acs.organomet.6b00155
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C30 H46 F3 O3 P2 Rh S'
_chemical_formula_sum            'C30 H46 F3 O3 P2 Rh S'
_chemical_formula_weight         708.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   31.7741(16)
_cell_length_b                   20.8238(9)
_cell_length_c                   34.6631(17)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.85
_cell_measurement_theta_min      2.55
_cell_volume                     22935.1(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'LinXTL v.  5.1.7'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1356
_diffrn_reflns_av_unetI/netI     0.1210
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            126927
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.499
_diffrn_reflns_theta_min         2.549
_exptl_absorpt_coefficient_mu    5.249
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8832
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         1.959
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1193
_refine_ls_number_reflns         19729
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1025P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10255
_reflns_number_total             19729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00155_si_002.cif
_cod_data_source_block           4_OTF_trans
_cod_depositor_comments
;

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum            'C90 H138 F9 O9 P6 Rh3 S3'
_cod_original_formula_weight         2125.73
_cod_original_formula_units_Z            8
_cod_database_code               4088529
_shelxl_version_number           2013-4
_shelx_res_checksum              33022
_shelx_hkl_checksum              6887