Rapid Access to Derivatized, Dimeric, Ring-Substituted Dichloro(cyclopentadienyl)rhodium(III) and Iridium(III) Complexes
Brown, Loren C.; Ressegue, Emily; Merola, Joseph S.; Organometallics 35 (2016) 4014–; doi:10.1021/acs.organomet.6b00580

data_4088971
_publ_section_title
;
 Rapid Access to Derivatized, Dimeric, Ring-Substituted
 Dichloro(cyclopentadienyl)rhodium(III) and Iridium(III) Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              4014
_journal_paper_doi               10.1021/acs.organomet.6b00580
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C34 H42 Cl4 Rh2'
_chemical_formula_sum            'C34 H42 Cl4 Rh2'
_chemical_formula_weight         798.29
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.933(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.19747(19)
_cell_length_b                   14.7032(3)
_cell_length_c                   14.0876(3)
_cell_measurement_reflns_used    17390
_cell_measurement_temperature    126(30)
_cell_measurement_theta_max      32.2370
_cell_measurement_theta_min      4.0420
_cell_volume                     1632.73(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      126(30)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0061
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
  1 omega   -4.00   74.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -       29.2190  -99.0000 -150.0000 78

  2 omega   -4.00   74.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -       29.2190  -99.0000  -60.0000 78

  3 omega   -4.00   74.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -       29.2190  -99.0000   90.0000 78

  4 omega -109.00  -35.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000 -120.0000 74

  5 omega -109.00  -35.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000  150.0000 74

  6 omega  -50.00   44.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   38.0000 -180.0000 94

  7 omega -105.00   37.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -19.0000    0.0000 142

  8 omega    6.00   92.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -       29.2190   57.0000   90.0000 86

  9 omega   -4.00  102.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -       29.2190   77.0000  150.0000 106

 10 omega  -50.00   44.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   38.0000   90.0000 94

 11 omega -102.00    4.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  -30.0000 106

 12 omega -100.00   -6.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000 -150.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0889272000
_diffrn_orient_matrix_UB_12      -0.0070997000
_diffrn_orient_matrix_UB_13      0.0122563000
_diffrn_orient_matrix_UB_21      -0.0120630000
_diffrn_orient_matrix_UB_22      -0.0345979000
_diffrn_orient_matrix_UB_23      -0.0363610000
_diffrn_orient_matrix_UB_31      0.0065544000
_diffrn_orient_matrix_UB_32      0.0328848000
_diffrn_orient_matrix_UB_33      -0.0356126000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40203
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.433
_diffrn_reflns_theta_min         3.605
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.3315
_exptl_crystal_size_mid          0.1372
_exptl_crystal_size_min          0.0917
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         5615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0203P)^2^+0.5356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4898
_reflns_number_total             5615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3m_lbx-031abs
_cod_original_cell_volume        1632.74(6)
_cod_database_code               4088971
_chemical_oxdiff_formula         'C34 H42 Cl4 Rh2'
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.04) H6B(0.04) H6C(0.04) H7A(0.042) H7B(0.042) H7C(0.042)
 H8A(0.041) H8B(0.041) H8C(0.041) H9A(0.036) H9B(0.036) H9C(0.036) H10A(0.021)
 H10B(0.021) H11A(0.02) H11B(0.02) H13(0.022) H14(0.025) H15(0.026) H16(0.026)
 H17(0.023)
 Fixed X: H6A(0.2475) H6B(0.4183) H6C(0.2477) H7A(-0.1133) H7B(-0.073)
 H7C(0.0328) H8A(-0.1159) H8B(0.021) H8C(-0.088) H9A(0.254) H9B(0.422)
 H9C(0.2502) H10A(0.5684) H10B(0.5598) H11A(0.3939) H11B(0.3814) H13(0.6832)
 H14(0.9476) H15(1.0428) H16(0.8694) H17(0.6042)
 Fixed Y: H6A(0.3662) H6B(0.4052) H6C(0.4015) H7A(0.4527) H7B(0.4891)
 H7C(0.4058) H8A(0.701) H8B(0.732) H8C(0.6416) H9A(0.7869) H9B(0.7658)
 H9C(0.7926) H10A(0.5407) H10B(0.6493) H11A(0.5453) H11B(0.6539) H13(0.4757)
 H14(0.492) H15(0.6364) H16(0.7627) H17(0.7471)
 Fixed Z: H6A(0.2885) H6B(0.2698) H6C(0.1811) H7A(0.2717) H7B(0.3828)
 H7C(0.3569) H8A(0.2932) H8B(0.3924) H8C(0.3915) H9A(0.2389) H9B(0.3256)
 H9C(0.3517) H10A(0.2616) H10B(0.2681) H11A(0.0946) H11B(0.1009) H13(0.1078)
 H14(0.0773) H15(0.046) H16(0.041) H17(0.0714)
;
_shelx_res_checksum              70871
_shelx_hkl_checksum              88322
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'