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_7042658
_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         'C27 H39 P Si3'
_chemical_formula_sum            'C27 H39 P Si3'
_chemical_formula_weight         478.82
_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             2017-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-21 deposited with the CCDC.
2017-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.735(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5658(11)
_cell_length_b                   15.6412(8)
_cell_length_c                   10.4063(5)
_cell_measurement_reflns_used    3927
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      72.3130
_cell_measurement_theta_min      5.1310
_cell_volume                     2849.4(3)
_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      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -28.00   51.00   1.0000    4.3900
omega____ theta____ kappa____ phi______ frames
    -       36.3926  -57.0000  -30.0000 79

  2 omega    4.00   69.00   1.0000    4.3900
omega____ theta____ kappa____ phi______ frames
    -       36.3926  -99.0000  -60.0000 65

  3 omega    3.00   73.00   1.0000    4.3900
omega____ theta____ kappa____ phi______ frames
    -       36.3926  -99.0000 -150.0000 70

  4 omega   49.00  106.00   1.0000   17.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -180.0000 57

  5 omega   55.00   82.00   1.0000   17.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 27

  6 omega   42.00  128.00   1.0000   17.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -180.0000 86

  7 omega   70.00  102.00   1.0000    4.3900
omega____ theta____ kappa____ phi______ frames
    -       36.3926   57.0000  -90.0000 32

  8 omega   38.00   68.00   1.0000    4.3900
omega____ theta____ kappa____ phi______ frames
    -       36.3926   57.0000  -90.0000 30

  9 omega   43.00   78.00   1.0000   17.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 35

 10 omega   76.00  177.00   1.0000   17.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   30.0000 101

 11 omega  112.00  166.00   1.0000   17.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 54

 12 omega   58.00  116.00   1.0000   17.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -30.0000 58

 13 omega   41.00   98.00   1.0000   17.5500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 57

 14 omega  -28.00   15.00   1.0000    4.3900
omega____ theta____ kappa____ phi______ frames
    -       36.3926  -77.0000   60.0000 43
;
_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      -0.0593013000
_diffrn_orient_matrix_UB_12      0.0275199000
_diffrn_orient_matrix_UB_13      0.0931782000
_diffrn_orient_matrix_UB_21      -0.0645609000
_diffrn_orient_matrix_UB_22      -0.0141363000
_diffrn_orient_matrix_UB_23      -0.1071845000
_diffrn_orient_matrix_UB_31      -0.0076178000
_diffrn_orient_matrix_UB_32      -0.0935169000
_diffrn_orient_matrix_UB_33      0.0435186000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8637
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        62.497
_diffrn_reflns_theta_max         62.497
_diffrn_reflns_theta_min         5.053
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62099
_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 colourless'
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1032
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.461
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.1044
_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^)+(0.1096P)^2^+18.8665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2609
_refine_ls_wR_factor_ref         0.2692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3869
_reflns_number_total             4505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00727b2.cif
_cod_data_source_block           mm104
_cod_database_code               7042658
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H P Si'
_reflns_odcompleteness_completeness 99.64
_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, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 Si1(H1), Si2(H2), Si3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C16(H16A,H16B), C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15),
 C21(H21), C22(H22), C23(H23), C24(H24)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              13280
_olex2_date_sample_data_collection 2017-02-15
_olex2_submission_special_instructions 'No special instructions were received'