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_4088969
_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         'C30 H50 Cl4 Rh2'
_chemical_formula_sum            'C30 H50 Cl4 Rh2'
_chemical_formula_weight         758.32
_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             2016-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.055(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1142(5)
_cell_length_b                   8.87820(17)
_cell_length_c                   20.4175(4)
_cell_measurement_reflns_used    16592
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      32.2660
_cell_measurement_theta_min      3.7580
_cell_volume                     3283.57(13)
_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      99.95(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 0.936
_diffrn_measurement_details
;
  1 omega -111.00  -76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  178.0000  150.0000 35

  2 omega -102.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  120.0000 106

  3 omega  -97.00  -59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000 -120.0000 38

  4 omega  -48.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   38.0000  -90.0000 92

  5 omega  -82.00    7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  114.0000   11.0000 89

  6 omega -104.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315    0.0000   90.0000 102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0155821000
_diffrn_orient_matrix_UB_12      -0.0339466000
_diffrn_orient_matrix_UB_13      -0.0282242000
_diffrn_orient_matrix_UB_21      0.0294437000
_diffrn_orient_matrix_UB_22      -0.0285216000
_diffrn_orient_matrix_UB_23      0.0192949000
_diffrn_orient_matrix_UB_31      -0.0205764000
_diffrn_orient_matrix_UB_32      -0.0664920000
_diffrn_orient_matrix_UB_33      0.0061149000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35727
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.410
_diffrn_reflns_theta_min         3.743
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.752
_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    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.3072
_exptl_crystal_size_mid          0.1967
_exptl_crystal_size_min          0.1702
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         10851
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0203P)^2^+2.7587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9700
_reflns_number_total             10851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3h_lbx-026
_cod_database_code               4088969
_chemical_oxdiff_formula         'C30 H50 Cl4 Rh2'
_chemical_oxdiff_usercomment     TGI11
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.041) H6B(0.041) H6C(0.041) H7A(0.046) H7B(0.046) H7C(0.046)
 H8A(0.053) H8B(0.053) H8C(0.053) H9A(0.049) H9B(0.049) H9C(0.049) H10A(0.031)
 H10B(0.031) H11A(0.035) H11B(0.035) H12A(0.048) H12B(0.048) H13A(0.046)
 H13B(0.046) H14A(0.073) H14B(0.073) H15A(0.083) H15B(0.083) H15C(0.083)
 H21A(0.032) H21B(0.032) H21C(0.032) H22A(0.042) H22B(0.042) H22C(0.042)
 H23A(0.054) H23B(0.054) H23C(0.054) H24A(0.064) H24B(0.064) H24C(0.064)
 H25A(0.031) H25B(0.031) H26A(0.031) H26B(0.031) H27C(0.038) H27D(0.038)
 H27A(0.038) H27B(0.038) H28A(0.078) H28B(0.078) H29A(0.093) H29B(0.093)
 H30A(0.13) H30B(0.13) H30C(0.13) H29C(0.047) H29D(0.047) H30D(0.091)
 H30E(0.091) H30F(0.091) H28C(0.039) H28D(0.039)
 Fixed X: H6A(0.6914) H6B(0.7414) H6C(0.7634) H7A(0.9017) H7B(0.9102)
 H7C(0.9638) H8A(0.9937) H8B(0.9687) H8C(0.9621) H9A(0.8527) H9B(0.8144)
 H9C(0.7665) H10A(0.6507) H10B(0.6692) H11A(0.6583) H11B(0.6457) H12A(0.5333)
 H12B(0.5442) H13A(0.525) H13B(0.5241) H14A(0.413) H14B(0.4137) H15A(0.3332)
 H15B(0.4004) H15C(0.3942) H21A(0.84) H21B(0.8619) H21C(0.9196) H22A(0.9908)
 H22B(0.9849) H22C(0.9907) H23A(0.9182) H23B(0.8589) H23C(0.8386) H24A(0.7092)
 H24B(0.6905) H24C(0.6584) H25A(0.7131) H25B(0.661) H26A(0.7187) H26B(0.6629)
 H27C(0.5738) H27D(0.6291) H27A(0.5675) H27B(0.6203) H28A(0.5702) H28B(0.6195)
 H29A(0.4744) H29B(0.476) H30A(0.5765) H30B(0.5159) H30C(0.5794) H29C(0.4915)
 H29D(0.5422) H30D(0.4798) H30E(0.5085) H30F(0.5637) H28C(0.5968) H28D(0.6473)
 Fixed Y: H6A(0.809) H6B(0.9485) H6C(0.8376) H7A(0.8348) H7B(0.9492)
 H7C(0.8113) H8A(0.637) H8B(0.7074) H8C(0.5333) H9A(0.4183) H9B(0.5445)
 H9C(0.4319) H10A(0.6097) H10B(0.5162) H11A(0.732) H11B(0.8318) H12A(0.7836)
 H12B(0.6107) H13A(0.8115) H13B(0.6355) H14A(0.8134) H14B(0.638) H15A(0.7163)
 H15B(0.7828) H15C(0.6085) H21A(0.1141) H21B(0.0029) H21C(0.1198) H22A(0.292)
 H22B(0.1971) H22C(0.3731) H23A(0.5162) H23B(0.4449) H23C(0.5854) H24A(0.5385)
 H24B(0.3843) H24C(0.4217) H25A(0.1664) H25B(0.2558) H26A(-0.0332) H26B(0.0553)
 H27C(0.0379) H27D(-0.0652) H27A(0.016) H27B(-0.0237) H28A(-0.146) H28B(-
 0.2503) H29A(-0.3026) H29B(-0.1762) H30A(-0.2796) H30B(-0.4053) H30C(-0.3993)
 H29C(-0.2009) H29D(-0.246) H30D(-0.4628) H30E(-0.4395) H30F(-0.4847) H28C(-
 0.2191) H28D(-0.2592)
 Fixed Z: H6A(0.3109) H6B(0.2953) H6C(0.3518) H7A(0.3412) H7B(0.2832)
 H7C(0.2888) H8A(0.2112) H8B(0.1444) H8C(0.1558) H9A(0.1203) H9B(0.0787)
 H9C(0.1197) H10A(0.2466) H10B(0.1835) H11A(0.1185) H11B(0.1808) H12A(0.1256)
 H12B(0.1368) H13A(0.2419) H13B(0.247) H14A(0.1895) H14B(0.1821) H15A(0.2642)
 H15B(0.3031) H15C(0.2921) H21A(0.3816) H21B(0.438) H21C(0.4117) H22A(0.4734)
 H22B(0.5379) H22C(0.5416) H23A(0.604) H23B(0.6505) H23C(0.6075) H24A(0.5742)
 H24B(0.6077) H24C(0.5382) H25A(0.4054) H25B(0.4529) H26A(0.4837) H26B(0.528)
 H27C(0.4411) H27D(0.4028) H27A(0.4578) H27B(0.3995) H28A(0.5254) H28B(0.4818)
 H29A(0.4774) H29B(0.4218) H30A(0.3788) H30B(0.383) H30C(0.4352) H29C(0.4353)
 H29D(0.3761) H30D(0.4112) H30E(0.4829) H30F(0.4272) H28C(0.5081) H28D(0.4478)
;
_shelx_res_checksum              85107
_shelx_hkl_checksum              52441
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'