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_4088967
_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      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                 96.9350(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.92156(10)
_cell_length_b                   16.4923(2)
_cell_length_c                   10.89610(13)
_cell_measurement_reflns_used    24230
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      32.2900
_cell_measurement_theta_min      4.1070
_cell_volume                     1413.10(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
  1 omega -102.00    4.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000 -180.0000 106

  2 omega  -63.00   43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000   60.0000 106

  3 omega -102.00    4.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -78.0000   97.0000 106

  4 omega  -63.00   43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000  -30.0000 106

  5 omega -105.00   37.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -19.0000 -180.0000 142

  6 omega -100.00   -6.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000  -30.0000 94

  7 omega -109.00  -35.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000 -180.0000 74

  8 omega -102.00    4.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  -90.0000 106

  9 omega -112.00  -32.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  178.0000   30.0000 80

 10 omega -102.00    4.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000   60.0000 106

 11 omega  -63.00   43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000  -90.0000 106

 12 omega -103.00    2.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -38.0000  120.0000 105

 13 omega  -53.00   41.00   1.0000    6.0000
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      -0.0502318000
_diffrn_orient_matrix_UB_12      -0.0342512000
_diffrn_orient_matrix_UB_13      -0.0197200000
_diffrn_orient_matrix_UB_21      -0.0011867000
_diffrn_orient_matrix_UB_22      0.0125377000
_diffrn_orient_matrix_UB_23      -0.0623680000
_diffrn_orient_matrix_UB_31      0.0748954000
_diffrn_orient_matrix_UB_32      -0.0227986000
_diffrn_orient_matrix_UB_33      -0.0046743000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            44438
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.469
_diffrn_reflns_theta_min         3.580
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.518
_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    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.5453
_exptl_crystal_size_mid          0.1978
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         4891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0125P)^2^+1.0409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4523
_reflns_number_total             4891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3e_lbx-027abs
_cod_database_code               4088967
_chemical_oxdiff_formula         'C26 H42 Cl4 Rh2'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.027) H6B(0.027) H6C(0.027) H7A(0.037) H7B(0.037) H7C(0.037)
 H8A(0.032) H8B(0.032) H8C(0.032) H9A(0.028) H9B(0.028) H9C(0.028) H10A(0.015)
 H10B(0.015) H11(0.018) H12A(0.028) H12B(0.028) H12C(0.028) H13A(0.042)
 H13B(0.042) H13C(0.042)
 Fixed X: H6A(0.5093) H6B(0.5082) H6C(0.6561) H7A(0.6868) H7B(0.5569)
 H7C(0.6592) H8A(0.4165) H8B(0.2222) H8C(0.2708) H9A(0.0909) H9B(-0.0271)
 H9C(0.0272) H10A(0.2988) H10B(0.1743) H11(-0.0317) H12A(-0.0507) H12B(-0.1204)
 H12C(0.0652) H13A(0.1831) H13B(0.0007) H13C(0.1571)
 Fixed Y: H6A(0.8073) H6B(0.809) H6C(0.762) H7A(0.6674) H7B(0.6282)
 H7C(0.5713) H8A(0.4777) H8B(0.4995) H8C(0.4525) H9A(0.5053) H9B(0.5653)
 H9C(0.5887) H10A(0.7718) H10B(0.6994) H11(0.7469) H12A(0.7897) H12B(0.8594)
 H12C(0.867) H13A(0.8848) H13B(0.8716) H13C(0.815)
 Fixed Z: H6A(0.3852) H6B(0.2383) H6C(0.3229) H7A(0.1684) H7B(0.0607)
 H7C(0.1629) H8A(0.1436) H8B(0.0981) H8C(0.226) H9A(0.3748) H9B(0.2866)
 H9C(0.4284) H10A(0.4962) H10B(0.5231) H11(0.3604) H12A(0.5653) H12B(0.4703)
 H12C(0.5457) H13A(0.3432) H13B(0.2652) H13C(0.2406)
;
_shelx_res_checksum              16995
_shelx_hkl_checksum              40045
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'