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_7042657
_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         'C42 H44 Cl P2 Rh Si2, 3(C4 H8 O)'
_chemical_formula_sum            'C54 H68 Cl O3 P2 Rh Si2'
_chemical_formula_weight         1021.56
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-02-21 deposited with the CCDC.
2017-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.939(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6490(6)
_cell_length_b                   17.2473(4)
_cell_length_c                   13.9539(4)
_cell_measurement_reflns_used    11481
_cell_measurement_temperature    100.46(10)
_cell_measurement_theta_max      28.8140
_cell_measurement_theta_min      2.8030
_cell_volume                     4966.7(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.46(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.8993
_diffrn_measurement_details
;
  1 omega  -10.00   82.00   1.0000   26.1950
omega____ theta____ kappa____ phi______ frames
    -       15.2374   77.0000  -90.0000 92

  2 omega  -51.00   40.00   1.0000   26.1950
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -77.0000  150.0000 91

  3 omega   -4.00   71.00   1.0000   26.1950
omega____ theta____ kappa____ phi______ frames
    -       15.2374   38.0000 -150.0000 75

  4 omega    7.00   50.00   1.0000   26.1950
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000   30.0000 43

  5 omega   35.00   87.00   1.0000   26.1950
omega____ theta____ kappa____ phi______ frames
    -       15.2374  178.0000   60.0000 52

  6 omega  -74.00  -44.00   1.0000   26.1950
omega____ theta____ kappa____ phi______ frames
    -      -16.1749  132.0000  -50.0000 30
;
_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      -0.0035014000
_diffrn_orient_matrix_UB_12      0.0352847000
_diffrn_orient_matrix_UB_13      0.0254457000
_diffrn_orient_matrix_UB_21      0.0341906000
_diffrn_orient_matrix_UB_22      0.0032631000
_diffrn_orient_matrix_UB_23      0.0051073000
_diffrn_orient_matrix_UB_31      0.0005495000
_diffrn_orient_matrix_UB_32      0.0208532000
_diffrn_orient_matrix_UB_33      -0.0437503000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20468
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.057
_diffrn_reflns_theta_min         2.777
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85175
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0368P)^2^+12.4019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5317
_reflns_number_total             5972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00727b2.cif
_cod_data_source_block           mm75
_cod_database_code               7042657
_chemical_oxdiff_formula         'C30 H30 P2 Si2 Rh'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
O2 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 2A with sigma of 0.05 and
sigma for terminal atoms of 0.1
3. Rigid body (RIGU) restrains
 O2, C26, C27, C28, C29
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Others
 Fixed Sof: O2(0.5) C26(0.5) H26A(0.5) H26B(0.5) C27(0.5) H27A(0.5) H27B(0.5)
 C28(0.5) H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5)
;
_shelx_res_checksum              61914
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-23
_olex2_submission_special_instructions 'No special instructions were received'