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_4088968
_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         'C28 H46 Cl4 Rh2, 2(C H Cl3)'
_chemical_formula_sum            'C30 H48 Cl10 Rh2'
_chemical_formula_weight         969.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 102.531(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8669(3)
_cell_length_b                   9.6420(2)
_cell_length_c                   17.4793(5)
_cell_measurement_reflns_used    8149
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.3040
_cell_measurement_theta_min      3.8760
_cell_volume                     1952.35(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 0.998
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
  1 omega  -32.00   31.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   57.0000   60.0000 63

  2 omega  -50.00   23.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   57.0000  -90.0000 73

  3 omega  -23.00    6.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -81.0000 -179.8674 29

  4 omega  -29.00    3.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -80.0000  -94.2924 32

  5 omega  -25.00    6.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -83.0000   53.5553 31

  6 omega -100.00   39.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315    0.0000   60.0000 139

  7 omega -106.00  -60.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000   60.0000 46

  8 omega -111.00  -59.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  178.0000 -120.0000 52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0018468000
_diffrn_orient_matrix_UB_12      -0.0486978000
_diffrn_orient_matrix_UB_13      0.0301150000
_diffrn_orient_matrix_UB_21      -0.0569201000
_diffrn_orient_matrix_UB_22      0.0215418000
_diffrn_orient_matrix_UB_23      0.0006505000
_diffrn_orient_matrix_UB_31      -0.0224513000
_diffrn_orient_matrix_UB_32      -0.0507618000
_diffrn_orient_matrix_UB_33      -0.0286497000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20750
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.492
_diffrn_reflns_theta_min         3.632
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.550
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.672
_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    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.4802
_exptl_crystal_size_mid          0.3026
_exptl_crystal_size_min          0.2062
_refine_diff_density_max         1.233
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         6508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0212P)^2^+0.5566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5389
_reflns_number_total             6508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3g_lbx-045abs
_cod_database_code               4088968
_chemical_oxdiff_formula         'C28 H46 Cl4 Rh2'
_chemical_oxdiff_usercomment     LBI101
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.036) H6B(0.036) H6C(0.036) H7A(0.035) H7B(0.035) H7C(0.035)
 H8A(0.04) H8B(0.04) H8C(0.04) H9A(0.043) H9B(0.043) H9C(0.043) H10A(0.028)
 H10B(0.028) H11A(0.023) H11B(0.023) H12A(0.03) H12B(0.03) H13A(0.031)
 H13B(0.031) H14A(0.047) H14B(0.047) H14C(0.047) H15(0.027)
 Fixed X: H6A(0.7842) H6B(0.8634) H6C(0.864) H7A(0.8525) H7B(0.8743)
 H7C(0.7857) H8A(0.6201) H8B(0.5931) H8C(0.4939) H9A(0.3852) H9B(0.4377)
 H9C(0.3886) H10A(0.6178) H10B(0.4937) H11A(0.6952) H11B(0.5678) H12A(0.6312)
 H12B(0.5083) H13A(0.6258) H13B(0.7201) H14A(0.5944) H14B(0.6054) H14C(0.4937)
 H15(0.3867)
 Fixed Y: H6A(0.4154) H6B(0.5485) H6C(0.4764) H7A(0.6017) H7B(0.7586)
 H7C(0.7256) H8A(0.852) H8B(0.9566) H8C(0.8562) H9A(0.7857) H9B(0.8529)
 H9C(0.6979) H10A(0.4589) H10B(0.532) H11A(0.6715) H11B(0.7352) H12A(0.4984)
 H12B(0.5738) H13A(0.6371) H13B(0.6995) H14A(0.8764) H14B(0.8754) H14C(0.8105)
 H15(0.2968)
 Fixed Z: H6A(0.2518) H6B(0.2791) H6C(0.1967) H7A(0.0847) H7B(0.1139)
 H7C(0.033) H8A(0.0076) H8B(0.0724) H8C(0.0263) H9A(0.1171) H9B(0.2009)
 H9C(0.1952) H10A(0.3007) H10B(0.2774) H11A(0.3653) H11B(0.3466) H12A(0.445)
 H12B(0.43) H13A(0.5535) H13B(0.5102) H14A(0.456) H14B(0.5489) H14C(0.4922)
 H15(0.1549)
;
_shelx_res_checksum              66041
_shelx_hkl_checksum              64915
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'