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_4088957
_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 Ir2'
_chemical_formula_sum            'C26 H42 Cl4 Ir2'
_chemical_formula_weight         880.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                109.693(4)
_cell_angle_beta                 100.752(3)
_cell_angle_gamma                92.206(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7695(3)
_cell_length_b                   8.8947(4)
_cell_length_c                   9.5445(3)
_cell_measurement_reflns_used    7928
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      32.2580
_cell_measurement_theta_min      3.9080
_cell_volume                     684.49(5)
_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(2)
_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 0.998
_diffrn_measurement_details
;
  1 omega -109.00  -35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000   60.0000 74

  2 omega -102.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000 -150.0000 106

  3 omega  -64.00   43.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   80.0000  -15.0000 107

  4 omega -102.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000   90.0000 106

  5 omega  -63.00   43.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000   90.0000 106

  6 omega -104.00   45.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315    0.0000 -180.0000 149

  7 omega -109.00  -49.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000  120.0000 60

  8 omega -100.00   -6.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000  -30.0000 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      -0.0577783000
_diffrn_orient_matrix_UB_12      -0.0470108000
_diffrn_orient_matrix_UB_13      0.0149902000
_diffrn_orient_matrix_UB_21      -0.0514941000
_diffrn_orient_matrix_UB_22      -0.0029503000
_diffrn_orient_matrix_UB_23      -0.0679056000
_diffrn_orient_matrix_UB_31      0.0295005000
_diffrn_orient_matrix_UB_32      -0.0710086000
_diffrn_orient_matrix_UB_33      -0.0410812000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12303
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        30.032
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         3.595
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.115
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_correction_T_min  0.099
_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    2.137
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.3332
_exptl_crystal_size_mid          0.2791
_exptl_crystal_size_min          0.1645
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.977
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         3995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0223P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3696
_reflns_number_total             3995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           2d_lbx-015abs
_cod_original_cell_volume        684.50(5)
_cod_database_code               4088957
_chemical_oxdiff_formula         'C26 H42 Cl4 Ir2'
_chemical_oxdiff_usercomment     'IrCp*butyl dimer'
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.029) H6B(0.029) H6C(0.029) H7A(0.028) H7B(0.028) H7C(0.028)
 H8A(0.024) H8B(0.024) H8C(0.024) H9A(0.022) H9B(0.022) H9C(0.022) H10A(0.021)
 H10B(0.021) H11A(0.023) H11B(0.023) H12A(0.021) H12B(0.021) H13A(0.03)
 H13B(0.03) H13C(0.03)
 Fixed X: H6A(0.4597) H6B(0.4998) H6C(0.6093) H7A(0.7019) H7B(0.6433)
 H7C(0.6427) H8A(0.4445) H8B(0.2925) H8C(0.2802) H9A(0.0514) H9B(-0.0017) H9C(-
 0.0229) H10A(0.1948) H10B(0.0491) H11A(0.0317) H11B(0.1822) H12A(-0.1024)
 H12B(0.0481) H13A(-0.1178) H13B(-0.1256) H13C(0.0302)
 Fixed Y: H6A(0.0565) H6B(0.2233) H6C(0.1688) H7A(0.3836) H7B(0.5299)
 H7C(0.5251) H8A(0.5874) H8B(0.6393) H8C(0.5161) H9A(0.3189) H9B(0.4062)
 H9C(0.2181) H10A(-0.0243) H10B(0.0445) H11A(0.0282) H11B(0.1505) H12A(0.2299)
 H12B(0.3521) H13A(0.2094) H13B(0.3875) H13C(0.3353)
 Fixed Z: H6A(0.8817) H6B(1.0145) H6C(0.8983) H7A(0.8152) H7B(0.9301)
 H7C(0.7643) H8A(0.6191) H8B(0.678) H8C(0.5129) H9A(0.4692) H9B(0.6217)
 H9C(0.5512) H10A(0.735) H10B(0.6659) H11A(0.9063) H11B(0.9823) H12A(0.8456)
 H12B(0.9243) H13A(1.0831) H13B(1.09) H13C(1.1609)
;
_shelx_res_checksum              74877
_shelx_hkl_checksum              43510
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'