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_4088970
_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         'C32 H38 Cl4 Rh2'
_chemical_formula_sum            'C32 H38 Cl4 Rh2'
_chemical_formula_weight         770.24
_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             2016-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.354(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6517(3)
_cell_length_b                   8.7062(3)
_cell_length_c                   20.4873(6)
_cell_measurement_reflns_used    6035
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      32.0700
_cell_measurement_theta_min      4.4500
_cell_volume                     1543.14(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -53.00  41.00   1.00    9.00    --  -29.53  57.00  30.00   94
  2  \w     13.00  43.00   1.00    9.00    --  -29.53  77.00 -90.00   30
  3  \w    -77.00 -38.00   1.00    9.00    --  -29.53 103.00-129.00   39
  4  \w   -112.00 -71.00   1.00    9.00    --  -29.53 178.00 -60.00   41
  5  \w    -99.00 -19.00   1.00    9.00    --  -29.53 -57.00 150.00   80
  6  \w   -108.00 -35.00   1.00    9.00    --  -29.53-178.00   0.00   73
  7  \w    -98.00  -6.00   1.00    9.00    --  -29.53 -57.00-120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0238964000
_diffrn_orient_matrix_UB_12      0.0008717000
_diffrn_orient_matrix_UB_13      0.0331896000
_diffrn_orient_matrix_UB_21      0.0010142000
_diffrn_orient_matrix_UB_22      0.0814293000
_diffrn_orient_matrix_UB_23      -0.0004883000
_diffrn_orient_matrix_UB_31      -0.0784280000
_diffrn_orient_matrix_UB_32      0.0013526000
_diffrn_orient_matrix_UB_33      0.0098706000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15797
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.390
_diffrn_reflns_theta_min         3.461
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.658
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         5101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0357
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4248
_reflns_number_total             5101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3l_lbx-022abs1
_cod_original_cell_volume        1543.13(8)
_cod_database_code               4088970
_chemical_oxdiff_formula         'C32 H38 Cl4 Rh2'
_chemical_oxdiff_usercomment     'Either LBI103, LBI92, LBi97'
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.028) H6B(0.028) H6C(0.028) H7A(0.029) H7B(0.029) H7C(0.029)
 H8A(0.028) H8B(0.028) H8C(0.028) H9A(0.031) H9B(0.031) H9C(0.031) H10A(0.021)
 H10B(0.021) H12(0.019) H13(0.02) H14(0.024) H15(0.023) H16(0.021)
 Fixed X: H6A(0.412) H6B(0.4174) H6C(0.3038) H7A(0.2893) H7B(0.3991)
 H7C(0.3636) H8A(0.6199) H8B(0.7028) H8C(0.8007) H9A(0.9452) H9B(0.9986)
 H9C(0.9725) H10A(0.6692) H10B(0.8187) H12(0.6866) H13(0.8299) H14(1.0867)
 H15(1.1956) H16(1.05)
 Fixed Y: H6A(0.5148) H6B(0.349) H6C(0.3795) H7A(0.1849) H7B(0.0391)
 H7C(0.1521) H8A(0.1407) H8B(0.0222) H8C(0.1569) H9A(0.3718) H9B(0.2801)
 H9C(0.4619) H10A(0.5871) H10B(0.6027) H12(0.3058) H13(0.2026) H14(0.282)
 H15(0.4686) H16(0.576)
 Fixed Z: H6A(0.7262) H6B(0.7598) H6C(0.6993) H7A(0.6254) H7B(0.6153)
 H7C(0.5555) H8A(0.4979) H8B(0.5465) H8C(0.5134) H9A(0.5547) H9B(0.6187)
 H9C(0.6219) H10A(0.7398) H10B(0.6946) H12(0.805) H13(0.8917) H14(0.909)
 H15(0.8411) H16(0.7559)
;
_shelx_res_checksum              91174
_shelx_hkl_checksum              349
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.047
_oxdiff_exptl_absorpt_empirical_full_min 0.941