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_4088963
_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         'C22 H34 Cl4 Rh2'
_chemical_formula_sum            'C22 H34 Cl4 Rh2'
_chemical_formula_weight         646.11
_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                 94.413(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7499(4)
_cell_length_b                   9.1382(2)
_cell_length_c                   19.8007(5)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    99.90(14)
_cell_measurement_theta_max      32.1180
_cell_measurement_theta_min      3.9570
_cell_volume                     2480.57(11)
_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      99.90(14)
_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 0.928
_diffrn_measurement_details
;
  1 omega -112.00  -42.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  178.0000  -30.0000 70

  2 omega  -68.00  -37.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000 -150.0000 31

  3 omega -100.00    4.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  150.0000 104

  4 omega -109.00  -74.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000  150.0000 35

  5 omega  -68.00   16.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   88.0000   -8.0000 84

  6 omega  -94.00   44.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   19.0000  -60.0000 138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0069150000
_diffrn_orient_matrix_UB_12      -0.0713617000
_diffrn_orient_matrix_UB_13      0.0128881000
_diffrn_orient_matrix_UB_21      -0.0298833000
_diffrn_orient_matrix_UB_22      -0.0179738000
_diffrn_orient_matrix_UB_23      -0.0296242000
_diffrn_orient_matrix_UB_31      0.0416696000
_diffrn_orient_matrix_UB_32      -0.0246763000
_diffrn_orient_matrix_UB_33      -0.0157143000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26396
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.367
_diffrn_reflns_theta_min         3.451
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.834
_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    1.730
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.3415
_exptl_crystal_size_mid          0.1662
_exptl_crystal_size_min          0.121
_refine_diff_density_max         2.203
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         8243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0245P)^2^+2.3835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6499
_reflns_number_total             8243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3a_lbx-023abs
_cod_original_cell_volume        2480.56(11)
_cod_database_code               4088963
_chemical_oxdiff_formula         'C22 H34 Cl4 Rh2'
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.039) H6B(0.039) H6C(0.039) H7A(0.042) H7B(0.042) H7C(0.042)
 H8A(0.046) H8B(0.046) H8C(0.046) H9A(0.05) H9B(0.05) H9C(0.05) H10A(0.031)
 H10B(0.031) H11A(0.056) H11B(0.056) H11C(0.056) H17A(0.03) H17B(0.03)
 H17C(0.03) H18A(0.042) H18B(0.042) H18C(0.042) H19A(0.042) H19B(0.042)
 H19C(0.052) H19D(0.052) H19E(0.052) H20A(0.046) H20B(0.046) H20C(0.046)
 H21A(0.039) H21B(0.039) H21C(0.039) H21D(0.031) H21E(0.031) H22A(0.037)
 H22B(0.037) H22C(0.037) H23A(0.07) H23B(0.07) H23C(0.07)
 Fixed X: H6A(0.568) H6B(0.6308) H6C(0.6585) H7A(0.8411) H7B(0.8513)
 H7C(0.931) H8A(0.9856) H8B(0.9669) H8C(0.9553) H9A(0.8236) H9B(0.7648)
 H9C(0.707) H10A(0.5328) H10B(0.5702) H11A(0.5158) H11B(0.4482) H11C(0.549)
 H17A(0.9268) H17B(0.8568) H17C(0.8288) H18A(0.6542) H18B(0.6304) H18C(0.5659)
 H19A(0.5268) H19B(0.5676) H19C(0.5271) H19D(0.5556) H19E(0.5702) H20A(0.7189)
 H20B(0.7675) H20C(0.8348) H21A(0.9605) H21B(0.9718) H21C(0.9877) H21D(0.9594)
 H21E(0.9867) H22A(0.5402) H22B(0.5889) H22C(0.4774) H23A(0.9825) H23B(1.0609)
 H23C(0.9577)
 Fixed Y: H6A(0.2164) H6B(0.0712) H6C(0.1799) H7A(0.1558) H7B(0.0414)
 H7C(0.1677) H8A(0.3628) H8B(0.2685) H8C(0.4427) H9A(0.5709) H9B(0.4565)
 H9C(0.5769) H10A(0.4184) H10B(0.5104) H11A(0.207) H11B(0.3382) H11C(0.3031)
 H17A(0.4981) H17B(0.5547) H17C(0.4108) H18A(0.4324) H18B(0.5838) H18C(0.5322)
 H19A(0.6867) H19B(0.7575) H19C(0.6819) H19D(0.8494) H19E(0.7789) H20A(0.8667)
 H20B(0.9784) H20C(0.8694) H21A(0.7353) H21B(0.8102) H21C(0.6377) H21D(0.7395)
 H21E(0.6326) H22A(0.9055) H22B(0.9781) H22C(0.9263) H23A(0.83) H23B(0.8548)
 H23C(0.9362)
 Fixed Z: H6A(0.6715) H6B(0.6871) H6C(0.6282) H7A(0.6405) H7B(0.7018)
 H7C(0.6965) H8A(0.7687) H8B(0.8346) H8C(0.8359) H9A(0.8699) H9B(0.9124)
 H9C(0.8664) H10A(0.736) H10B(0.8018) H11A(0.8061) H11B(0.8286) H11C(0.8714)
 H17A(0.3979) H17B(0.335) H17C(0.3752) H18A(0.3673) H18B(0.329) H18C(0.3885)
 H19A(0.4667) H19B(0.5369) H19C(0.4732) H19D(0.4618) H19E(0.5358) H20A(0.5937)
 H20B(0.5439) H20C(0.5902) H21A(0.5466) H21B(0.4746) H21C(0.4836) H21D(0.5469)
 H21E(0.4873) H22A(0.4129) H22B(0.4809) H22C(0.477) H23A(0.4133) H23B(0.4762)
 H23C(0.4738)
;
_shelx_res_checksum              26829
_shelx_hkl_checksum              25935
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'