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_4088965
_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         'C24 H38 Cl4 Rh2'
_chemical_formula_sum            'C24 H38 Cl4 Rh2'
_chemical_formula_weight         674.16
_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                 103.6785(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.82203(14)
_cell_length_b                   8.85285(13)
_cell_length_c                   17.2213(3)
_cell_measurement_reflns_used    16459
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.4010
_cell_measurement_theta_min      4.2910
_cell_volume                     1306.84(4)
_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      100.00(10)
_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 0.958
_diffrn_measurement_details
;
  1 omega  -63.00   43.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878   77.0000  -60.0000 106

  2 omega  -25.00    6.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  -82.0000  177.7051 31

  3 omega -100.00   -6.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  -57.0000  150.0000 94

  4 omega -112.00  -32.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  178.0000  -90.0000 80

  5 omega  -93.00   -1.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  131.0000   27.5025 92

  6 omega -105.00   45.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878    0.0000  -30.0000 150

  7 omega  -25.00    7.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  -83.0000  -51.5874 32

  8 omega -109.00  -35.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878 -178.0000   60.0000 74

  9 omega -102.00    3.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  -77.0000   60.0000 105

 10 omega -100.00   -6.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  -57.0000 -150.0000 94

 11 omega -100.00   -6.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  -57.0000  -90.0000 94

 12 omega -109.00  -78.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878 -178.0000  120.0000 31

 13 omega  -53.00   41.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878   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      -0.0379192000
_diffrn_orient_matrix_UB_12      -0.0709027000
_diffrn_orient_matrix_UB_13      -0.0012250000
_diffrn_orient_matrix_UB_21      0.0671406000
_diffrn_orient_matrix_UB_22      -0.0303562000
_diffrn_orient_matrix_UB_23      0.0264607000
_diffrn_orient_matrix_UB_31      -0.0300738000
_diffrn_orient_matrix_UB_32      0.0216740000
_diffrn_orient_matrix_UB_33      0.0330814000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32780
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.482
_diffrn_reflns_theta_min         3.715
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.682
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.689
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       irregular
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.3153
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.1227
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         4532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0138P)^2^+0.7113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4119
_reflns_number_total             4532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3b_lbx-050abs
_cod_database_code               4088965
_chemical_oxdiff_formula         'C24 H38 Cl4 Rh2'
_chemical_oxdiff_usercomment     ERI33
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.022) H6B(0.022) H6C(0.022) H7A(0.019) H7B(0.019) H7C(0.019)
 H8A(0.019) H8B(0.019) H8C(0.019) H9A(0.022) H9B(0.022) H9C(0.022) H10A(0.016)
 H10B(0.016) H11A(0.019) H11B(0.019) H12A(0.035) H12B(0.035) H12C(0.035)
 Fixed X: H6A(0.5523) H6B(0.7098) H6C(0.7) H7A(0.4993) H7B(0.5497) H7C(0.4318)
 H8A(0.7221) H8B(0.8073) H8C(0.6225) H9A(1.0487) H9B(1.0643) H9C(0.9426)
 H10A(1.0147) H10B(0.8946) H11A(1.0232) H11B(1.1394) H12A(1.2483) H12B(1.2657)
 H12C(1.1328)
 Fixed Y: H6A(0.5336) H6B(0.5577) H6C(0.4276) H7A(0.9518) H7B(0.8578)
 H7C(0.7853) H8A(1.0087) H8B(1.0784) H8C(1.0531) H9A(0.6979) H9B(0.8648)
 H9C(0.8316) H10A(0.4804) H10B(0.3915) H11A(0.4923) H11B(0.3911) H12A(0.613)
 H12B(0.615) H12C(0.7137)
 Fixed Z: H6A(0.2013) H6B(0.2687) H6C(0.2032) H7A(0.1419) H7B(0.2233)
 H7C(0.1473) H8A(-0.0043) H8B(0.0806) H8C(0.0588) H9A(0.0289) H9B(0.0657) H9C(-
 0.0174) H10A(0.0911) H10B(0.1311) H11A(0.2592) H11B(0.2225) H12A(0.181)
 H12B(0.2756) H12C(0.2184)
;
_shelx_res_checksum              10257
_shelx_hkl_checksum              74466
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'