Synthesis and characterization of rhodium, iridium, and palladium complexes of a diarylamido-based PNSb pincer ligand.
Kosanovich, Alex J.; Jordan, Aldo M.; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11619–11624; doi:10.1039/c8dt02207k

data_7047142
_publ_section_title
;
 Synthesis and characterization of rhodium, iridium, and palladium
 complexes of a diarylamido-based PNSb pincer ligand.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11619
_journal_page_last               11624
_journal_paper_doi               10.1039/c8dt02207k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C33 H36 N O P Rh Sb'
_chemical_formula_sum            'C33 H36 N O P Rh Sb'
_chemical_formula_weight         718.26
_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             2017-10-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-05-16 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.0040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5285(2)
_cell_length_b                   14.0615(3)
_cell_length_c                   20.1189(4)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      61.954
_cell_measurement_theta_min      3.836
_cell_volume                     2976.71(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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      110.0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.1114
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56253
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        54.985
_diffrn_reflns_theta_max         54.985
_diffrn_reflns_theta_min         3.836
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.382
_exptl_absorpt_correction_T_max  0.3766
_exptl_absorpt_correction_T_min  0.2557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1292 before and 0.0713 after correction. The Ratio of minimum to maximum transmission is 0.6790. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.021
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         3662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0388P)^2^+3.2014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3043
_reflns_number_total             3662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02207k2.cif
_cod_data_source_block           amj017
_cod_depositor_comments          'Adding full bibliography for 7047142.cif.'
_cod_database_code               7047142
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.781
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C22(H22), C12(H12), C24(H24), C23(H23), C32(H32), C3(H3), C9(H9),
 C5(H5), C26(H26), C6(H6), C30(H30), C28(H28), C31(H31), C25(H25), C29(H29)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C7(H7A,H7B,H7C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              25593
_olex2_submission_special_instructions 'No special instructions were received'