Oxidative formation of phosphinyl radicals from a trigonal pyramidal terminal phosphide Rh(i) complex, with an unusually long Rh-P bond.
Fischbach, Urs; Trincado, M.; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3443–3448; doi:10.1039/c7dt00070g

data_7041991
_publ_section_title
;
 Oxidative formation of phosphinyl radicals from a trigonal pyramidal
 terminal phosphide Rh(i) complex, with an unusually long Rh-P bond.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3443
_journal_page_last               3448
_journal_paper_doi               10.1039/c7dt00070g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C57 H43 O P2 Rh, C H2 Cl2'
_chemical_formula_sum            'C58 H45 Cl2 O P2 Rh'
_chemical_formula_weight         993.69
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-01-06 deposited with the CCDC.
2017-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5568(8)
_cell_length_b                   17.6715(12)
_cell_length_c                   22.3047(15)
_cell_measurement_temperature    200(2)
_cell_volume                     4495.0(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'CMOS 100-Bruker Area Detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51483
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.984
_diffrn_reflns_theta_min         1.478
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_correction_T_min  0.8232
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2008/1 Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         13321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+3.1621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10822
_reflns_number_total             13321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00070g2.cif
_cod_data_source_block           sadp21n
_cod_depositor_comments
'Adding full bibliography for 7041989--7041991.cif.'
_cod_database_code               7041991
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.823
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31), C4(H4), C35(H35), C5(H5), C20(H20), C19(H19), C1(H1), C16(H16),
 C34(H34)
2.b Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B)
2.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C23(H23), C26(H26), C12(H12), C43(H43), C40(H40), C39(H39),
 C15(H15), C51(H51), C30(H30), C42(H42), C45(H45), C38(H38), C11(H11), C8(H8),
 C13(H13), C14(H14), C57(H57), C44(H44), C25(H25), C24(H24), C47(H47), C29(H29),
  C48(H48), C28(H28), C27(H27), C10(H10), C53(H53), C9(H9), C49(H49), C56(H56),
 C50(H50), C55(H55), C54(H54)
;
_shelx_res_checksum              29310
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'