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_4088964
_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, 2(C H2 Cl2)'
_chemical_formula_sum            'C26 H42 Cl8 Rh2'
_chemical_formula_weight         844.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                81.339(5)
_cell_angle_beta                 84.115(5)
_cell_angle_gamma                71.983(6)
_cell_formula_units_Z            1
_cell_length_a                   8.7683(5)
_cell_length_b                   9.0638(6)
_cell_length_c                   10.9372(6)
_cell_measurement_reflns_used    5393
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.9010
_cell_measurement_theta_min      4.2440
_cell_volume                     815.73(9)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0061
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_details
;
  1 omega  -53.00   38.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   57.0000  -30.0000 91

  2 omega  -88.00    5.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  123.0000   70.0000 93

  3 omega  -48.00   35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   38.0000   90.0000 83

  4 omega  -94.00  -68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  -60.0000 26

  5 omega  -24.00    3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  -60.0000 27

  6 omega -100.00   -6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000 -180.0000 94

  7 omega -100.00  -71.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000  -60.0000 29

  8 omega -100.00   -6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000   30.0000 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      -0.0378774000
_diffrn_orient_matrix_UB_12      0.0272743000
_diffrn_orient_matrix_UB_13      0.0562563000
_diffrn_orient_matrix_UB_21      0.0627266000
_diffrn_orient_matrix_UB_22      -0.0555267000
_diffrn_orient_matrix_UB_23      0.0333022000
_diffrn_orient_matrix_UB_31      0.0435022000
_diffrn_orient_matrix_UB_32      0.0552574000
_diffrn_orient_matrix_UB_33      -0.0066991000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10558
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.446
_diffrn_reflns_theta_min         3.664
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.683
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.649
_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    1.718
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.4101
_exptl_crystal_size_mid          0.1635
_exptl_crystal_size_min          0.1034
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         5333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0171P)^2^+0.0299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4636
_reflns_number_total             5333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3b_lbx-017abs
_cod_database_code               4088964
_chemical_oxdiff_formula         'C13 H21 Cl4 Rh'
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.022) H6B(0.022) H6C(0.022) H7A(0.021) H7B(0.021) H7C(0.021)
 H8A(0.022) H8B(0.022) H8C(0.022) H9A(0.022) H9B(0.022) H9C(0.022) H10A(0.017)
 H10B(0.017) H11A(0.022) H11B(0.022) H12A(0.04) H12B(0.04) H12C(0.04)
 H13A(0.045) H13B(0.045)
 Fixed X: H6A(0.6236) H6B(0.5452) H6C(0.7198) H7A(0.9063) H7B(0.7427)
 H7C(0.7373) H8A(1.0488) H8B(0.8837) H8C(0.9404) H9A(0.997) H9B(0.8301)
 H9C(0.8482) H10A(0.5883) H10B(0.673) H11A(0.8375) H11B(0.9205) H12A(0.6648)
 H12B(0.7478) H12C(0.8486) H13A(0.3888) H13B(0.2586)
 Fixed Y: H6A(-0.095) H6B(-0.039) H6C(-0.1639) H7A(0.0208) H7B(0.1559) H7C(-
 0.0128) H8A(0.3072) H8B(0.4427) H8C(0.3004) H9A(0.3251) H9B(0.3668)
 H9C(0.4675) H10A(0.0932) H10B(0.2163) H11A(-0.1108) H11B(0.0128) H12A(-0.0694)
 H12B(0.054) H12C(-0.1269) H13A(0.4777) H13B(0.3845)
 Fixed Z: H6A(0.5604) H6B(0.6906) H6C(0.6833) H7A(0.3499) H7B(0.319)
 H7C(0.3845) H8A(0.459) H8B(0.4334) H8C(0.3521) H9A(0.7214) H9B(0.8024)
 H9C(0.6713) H10A(0.8559) H10B(0.8847) H11A(0.8787) H11B(0.9096) H12A(1.061)
 H12B(1.0918) H12C(1.096) H13A(0.8605) H13B(0.8757)
;
_shelx_res_checksum              5284
_shelx_hkl_checksum              67866
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'