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_4088966
_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         'C26 H42 Cl4 Rh2'
_chemical_formula_sum            'C26 H42 Cl4 Rh2'
_chemical_formula_weight         702.21
_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             2015-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                74.904(4)
_cell_angle_beta                 76.432(5)
_cell_angle_gamma                82.203(4)
_cell_formula_units_Z            1
_cell_length_a                   8.5876(5)
_cell_length_b                   8.7956(4)
_cell_length_c                   9.9373(5)
_cell_measurement_reflns_used    10578
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.3480
_cell_measurement_theta_min      4.1690
_cell_volume                     702.24(7)
_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 0.998
_diffrn_measurement_details
;
  1 omega -100.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000   90.0000 94

  2 omega -109.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000  120.0000 74

  3 omega -112.00  -32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  178.0000  -60.0000 80

  4 omega -109.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000 -180.0000 74

  5 omega -112.00  -32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  178.0000   60.0000 80

  6 omega  -90.00    2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  126.0000  -92.4384 92

  7 omega -105.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -19.0000  120.0000 142

  8 omega  -25.00    7.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -83.0000 -126.0037 32

  9 omega  -26.00    6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -81.0000    8.7638 32

 10 omega -100.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000   30.0000 94

 11 omega  -53.00   40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   59.0000   97.0000 93

 12 omega -100.00  -19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000 -180.0000 81

 13 omega -102.00    4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  -30.0000 106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0701355000
_diffrn_orient_matrix_UB_12      0.0314252000
_diffrn_orient_matrix_UB_13      -0.0469739000
_diffrn_orient_matrix_UB_21      -0.0458854000
_diffrn_orient_matrix_UB_22      0.0710302000
_diffrn_orient_matrix_UB_23      -0.0242831000
_diffrn_orient_matrix_UB_31      0.0155182000
_diffrn_orient_matrix_UB_32      0.0314317000
_diffrn_orient_matrix_UB_33      0.0540106000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6808
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93946
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description
;
;
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.3028
_exptl_crystal_size_mid          0.2191
_exptl_crystal_size_min          0.1194
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         6808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0324P)^2^+0.5587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5940
_reflns_number_total             6808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3d_lbx-020abs1
_cod_database_code               4088966
_chemical_oxdiff_formula         'C26 H42 Cl4 Rh2'
_chemical_oxdiff_usercomment     LBI90
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.031) H6B(0.031) H6C(0.031) H7A(0.031) H7B(0.031) H7C(0.031)
 H8A(0.03) H8B(0.03) H8C(0.03) H9A(0.031) H9B(0.031) H9C(0.031) H10A(0.021)
 H10B(0.021) H11A(0.018) H11B(0.018) H12A(0.021) H12B(0.021) H13A(0.028)
 H13B(0.028) H13C(0.028)
 Fixed X: H6A(0.5073) H6B(0.4588) H6C(0.3636) H7A(0.3202) H7B(0.4265)
 H7C(0.3773) H8A(0.624) H8B(0.738) H8C(0.8137) H9A(0.9838) H9B(1.0543)
 H9C(1.0288) H10A(0.7531) H10B(0.9141) H11A(0.8294) H11B(0.9926) H12A(1.0745)
 H12B(0.9134) H13A(1.1611) H13B(0.999) H13C(1.1272)
 Fixed Y: H6A(0.3359) H6B(0.1598) H6C(0.3052) H7A(0.1298) H7B(-0.0156)
 H7C(0.1385) H8A(0.1376) H8B(-0.0068) H8C(0.1511) H9A(0.3118) H9B(0.1798)
 H9C(0.3606) H10A(0.4261) H10B(0.4292) H11A(0.1546) H11B(0.1637) H12A(0.3557)
 H12B(0.3391) H13A(0.0905) H13B(0.0716) H13C(0.1868)
 Fixed Z: H6A(0.5148) H6B(0.5398) H6C(0.4501) H7A(0.31) H7B(0.2566)
 H7C(0.1431) H8A(-0.0431) H8B(0.0255) H8C(-0.0744) H9A(-0.0261) H9B(0.0937)
 H9C(0.1035) H10A(0.4352) H10B(0.314) H11A(0.5407) H11B(0.4229) H12A(0.5175)
 H12B(0.6384) H13A(0.6103) H13B(0.7298) H13C(0.7318)
;
_shelx_res_checksum              12691
_shelx_hkl_checksum              77056
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'