A family of rhodium and iridium complexes with semirigid benzylsilyl phosphines: from bidentate to tetradentate coordination modes
Corona-González, María Vicky; Zamora-Moreno, Julio; Cuevas-Chávez, Cynthia A.; Rufino-Felipe, Ernesto; Mothes-Martin, Emmanuelle; Coppel, Yannick; Muñoz-Hernández, Miguel A.; Vendier, Laure; Flores-Alamo, Marcos; Grellier, Mary; Sabo-Etienne, Sylviane; Montiel-Palma, Virginia; Dalton Trans.  (2017) –; doi:10.1039/C7DT00727B

data_7042660
_publ_section_title
;
 A family of rhodium and iridium complexes with semirigid benzylsilyl
 phosphines: from bidentate to tetradentate coordination modes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00727B
_journal_year                    2017
_chemical_formula_moiety         'C48 H58 Cl2 P2 Rh2 Si4, 2(C6 H6)'
_chemical_formula_sum            'C60 H70 Cl2 P2 Rh2 Si4'
_chemical_formula_weight         1242.18
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-21 deposited with the CCDC.
2017-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.2606(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.74490(13)
_cell_length_b                   21.9235(2)
_cell_length_c                   12.01200(13)
_cell_measurement_reflns_used    6869
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      72.5980
_cell_measurement_theta_min      3.9580
_cell_volume                     2937.20(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega   45.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8926 -125.0000   60.0000 43

  2 omega   43.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8926 -125.0000    0.0000 28

  3 omega   39.00   96.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8926   77.0000  120.0000 57

  4 omega   22.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8926   38.0000  -30.0000 66

  5 omega   56.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8926   57.0000   90.0000 35

  6 omega  -29.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8926  -38.0000  150.0000 81

  7 omega   58.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 33

  8 omega   41.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 53

  9 omega   58.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 26

 10 omega   46.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -90.0000 57

 11 omega   40.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  120.0000 49

 12 omega   60.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 28

 13 omega   62.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 53

 14 omega  100.00  127.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -30.0000 27

 15 omega   81.00  164.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  150.0000 83

 16 omega  106.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   90.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0092460000
_diffrn_orient_matrix_UB_12      0.0700859000
_diffrn_orient_matrix_UB_13      0.0065601000
_diffrn_orient_matrix_UB_21      -0.1186113000
_diffrn_orient_matrix_UB_22      0.0051182000
_diffrn_orient_matrix_UB_23      -0.1015710000
_diffrn_orient_matrix_UB_31      -0.0702388000
_diffrn_orient_matrix_UB_32      0.0006408000
_diffrn_orient_matrix_UB_33      0.0887932000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11269
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.654
_diffrn_reflns_theta_min         3.963
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.956
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0436P)^2^+0.9865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5259
_reflns_number_total             5700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00727b2.cif
_cod_data_source_block           mm69
_cod_original_cell_volume        2937.21(6)
_cod_database_code               7042660
_chemical_oxdiff_formula         'C30 H30 P2 Si4 Rh2'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29)
2.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              32613
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-09
_olex2_submission_special_instructions 'No special instructions were received'