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_4088961
_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 Ir2'
_chemical_formula_sum            'C34 H42 Cl4 Ir2'
_chemical_formula_weight         976.87
_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                 105.5813(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.24614(13)
_cell_length_b                   14.78789(19)
_cell_length_c                   14.1153(2)
_cell_measurement_reflns_used    20061
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.1200
_cell_measurement_theta_min      4.0450
_cell_volume                     1658.01(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    '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 0.998
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega -112.00  -32.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  178.0000   90.0000 80

  2 omega -102.00    4.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000   60.0000 106

  3 omega  -50.00   44.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   38.0000 -150.0000 94

  4 omega -102.00    4.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  -90.0000 106

  5 omega  -67.00   40.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   86.0000   16.0000 107

  6 omega -104.00   45.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315    0.0000   30.0000 149

  7 omega -109.00  -35.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000    0.0000 74

  8 omega -100.00   -6.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000  -60.0000 94

  9 omega -109.00  -35.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000 -180.0000 74

 10 omega -102.00   -9.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  150.0000 93

 11 omega -100.00   -6.00   1.0000   13.0000
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      0.0111540000
_diffrn_orient_matrix_UB_12      0.0313969000
_diffrn_orient_matrix_UB_13      -0.0357179000
_diffrn_orient_matrix_UB_21      0.0607476000
_diffrn_orient_matrix_UB_22      -0.0289397000
_diffrn_orient_matrix_UB_23      -0.0113723000
_diffrn_orient_matrix_UB_31      -0.0645004000
_diffrn_orient_matrix_UB_32      -0.0218509000
_diffrn_orient_matrix_UB_33      -0.0362718000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.951
_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            41554
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.399
_diffrn_reflns_theta_min         3.576
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21773
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.4688
_exptl_crystal_size_mid          0.0949
_exptl_crystal_size_min          0.087
_refine_diff_density_max         3.246
_refine_diff_density_min         -1.750
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         5671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0254P)^2^+1.8645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5073
_reflns_number_total             5671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           2m_lbx-028abs
_cod_original_cell_volume        1658.00(5)
_cod_database_code               4088961
_chemical_oxdiff_formula         'C34 H42 Cl4 Ir2'
_chemical_oxdiff_usercomment     LBI94
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.052) H6B(0.052) H6C(0.052) H7A(0.054) H7B(0.054) H7C(0.054)
 H8A(0.05) H8B(0.05) H8C(0.05) H9A(0.041) H9B(0.041) H9C(0.041) H10A(0.025)
 H10B(0.025) H11A(0.023) H11B(0.023) H13(0.025) H14(0.028) H15(0.028) H16(0.03)
 H17(0.026)
 Fixed X: H6A(0.7483) H6B(0.5779) H6C(0.7448) H7A(1.1146) H7B(1.064)
 H7C(0.9665) H8A(1.1166) H8B(0.9823) H8C(1.0899) H9A(0.7622) H9B(0.5883)
 H9C(0.7538) H10A(0.4309) H10B(0.4442) H11A(0.6035) H11B(0.6168) H13(0.3132)
 H14(0.0511) H15(-0.0421) H16(0.1318) H17(0.3958)
 Fixed Y: H6A(0.3648) H6B(0.4052) H6C(0.4018) H7A(0.4523) H7B(0.4817)
 H7C(0.4004) H8A(0.6957) H8B(0.7257) H8C(0.6352) H9A(0.7847) H9B(0.7656)
 H9C(0.7896) H10A(0.5431) H10B(0.6508) H11A(0.5473) H11B(0.6552) H13(0.4795)
 H14(0.4959) H15(0.6395) H16(0.765) H17(0.7486)
 Fixed Z: H6A(0.7183) H6B(0.7346) H6C(0.8242) H7A(0.7307) H7B(0.6174)
 H7C(0.6531) H8A(0.7093) H8B(0.6098) H8C(0.6124) H9A(0.7663) H9B(0.6853)
 H9C(0.6518) H10A(0.7415) H10B(0.7348) H11A(0.9082) H11B(0.9015) H13(0.8933)
 H14(0.9229) H15(0.9572) H16(0.962) H17(0.9325)
;
_shelx_res_checksum              93402
_shelx_hkl_checksum              79789
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'