Metal- and Ligand-Centered Reactivity of meta-Carboranyl-Backbone Pincer Complexes of Rhodium
Eleazer, Bennett J.; Smith, Mark D.; Peryshkov, Dmitry V.; Organometallics 35 (2016) 106–; doi:10.1021/acs.organomet.5b00807

data_4088020
_publ_section_title
;
 Metal- and Ligand-Centered Reactivity of meta-Carboranyl-Backbone Pincer
 Complexes of Rhodium
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              106
_journal_paper_doi               10.1021/acs.organomet.5b00807
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C22 H45 B10 I N O2 P2 Rh, C6 D6'
_chemical_formula_sum            'C28 H45 B10 D6 I N O2 P2 Rh'
_chemical_formula_weight         839.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                76.180(2)
_cell_angle_beta                 72.455(2)
_cell_angle_gamma                80.535(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6949(5)
_cell_length_b                   11.3884(6)
_cell_length_c                   16.3856(8)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.46
_cell_volume                     1838.57(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_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            96810
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.900
_diffrn_reflns_theta_max         27.902
_diffrn_reflns_theta_min         2.456
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  0.4917
_exptl_absorpt_correction_T_min  0.4707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0683 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.9573.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00113(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         8733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0147P)^2^+1.9168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7228
_reflns_number_total             8733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00807_si_001.cif
_cod_data_source_block           be291a_0m
_cod_database_code               4088020
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.895
_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:
 C11(H11), C14(H14), C21(H21), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5A), C6(H6A), C7(H7A), C8(H8A), C31(D31), C32(D32), C33(D33),
 C34(D34), C35(D35), C36(D36)
2.c Idealised Me refined as rotating group:
 C10(H10B,H10C,H10D), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              72477
_shelx_hkl_checksum              47875
_olex2_submission_special_instructions 'No special instructions were received'