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_4088960
_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 Ir2, 2(C H Cl3)'
_chemical_formula_sum            'C30 H48 Cl10 Ir2'
_chemical_formula_weight         1147.58
_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
_audit_creation_date             2016-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.795(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8539(3)
_cell_length_b                   9.6544(3)
_cell_length_c                   17.4993(5)
_cell_measurement_reflns_used    6041
_cell_measurement_temperature    100.1(7)
_cell_measurement_theta_max      32.0010
_cell_measurement_theta_min      4.1390
_cell_volume                     1960.37(10)
_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      100.1(7)
_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 0.916
_diffrn_measurement_details
;
  1 omega  -95.00  -59.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000  -90.0000 36

  2 omega  -76.00   41.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315    0.0000 -120.0000 117

  3 omega -103.00   -5.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -38.0000 -120.0000 98

  4 omega -102.00  -67.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000  150.0000 35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0081276000
_diffrn_orient_matrix_UB_12      0.0335061000
_diffrn_orient_matrix_UB_13      0.0345365000
_diffrn_orient_matrix_UB_21      0.0603193000
_diffrn_orient_matrix_UB_22      -0.0014238000
_diffrn_orient_matrix_UB_23      0.0148130000
_diffrn_orient_matrix_UB_31      0.0054594000
_diffrn_orient_matrix_UB_32      0.0654077000
_diffrn_orient_matrix_UB_33      -0.0173791000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12825
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         32.307
_diffrn_reflns_theta_min         3.641
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.484
_exptl_absorpt_correction_T_max  0.431
_exptl_absorpt_correction_T_min  0.223
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.3567
_exptl_crystal_size_mid          0.2666
_exptl_crystal_size_min          0.1437
_refine_diff_density_max         1.671
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         6392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0160P)^2^+1.2210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5336
_reflns_number_total             6392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           2g_lbx-018abs
_cod_original_cell_volume        1960.36(9)
_cod_database_code               4088960
_chemical_oxdiff_formula         'C28 H46 Cl4 Ir2'
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.038) H6B(0.038) H6C(0.038) H7A(0.036) H7B(0.036) H7C(0.036)
 H8A(0.041) H8B(0.041) H8C(0.041) H9A(0.044) H9B(0.044) H9C(0.044) H10A(0.031)
 H10B(0.031) H11A(0.027) H11B(0.027) H12A(0.032) H12B(0.032) H13A(0.036)
 H13B(0.036) H14A(0.05) H14B(0.05) H14C(0.05) H15(0.029)
 Fixed X: H6A(0.8677) H6B(0.857) H6C(0.7822) H7A(0.7888) H7B(0.8746)
 H7C(0.8566) H8A(0.4996) H8B(0.6095) H8C(0.6207) H9A(0.3875) H9B(0.437)
 H9C(0.3869) H10A(0.4903) H10B(0.6122) H11A(0.5697) H11B(0.695) H12A(0.6258)
 H12B(0.5058) H13A(0.6236) H13B(0.7206) H14A(0.5996) H14B(0.4993) H14C(0.6152)
 H15(0.6123)
 Fixed Y: H6A(0.5163) H6B(0.4527) H6C(0.5854) H7A(0.2768) H7B(0.2371)
 H7C(0.396) H8A(0.1282) H8B(0.0396) H8C(0.1494) H9A(0.2965) H9B(0.1418)
 H9C(0.2103) H10A(0.4602) H10B(0.5382) H11A(0.2614) H11B(0.3302) H12A(0.5002)
 H12B(0.4191) H13A(0.3638) H13B(0.3064) H14A(0.1231) H14B(0.1819) H14C(0.1226)
 H15(0.2969)
 Fixed Z: H6A(0.7) H6B(0.7826) H6C(0.7489) H7A(0.5333) H7B(0.6134) H7C(0.5877)
 H8A(0.5315) H8B(0.5726) H8C(0.506) H9A(0.6946) H9B(0.6997) H9C(0.6164)
 H10A(0.7784) H10B(0.8002) H11A(0.8475) H11B(0.8648) H12A(0.9442) H12B(0.9309)
 H13A(1.0527) H13B(1.0096) H14A(0.9563) H14B(0.9961) H14C(1.0493) H15(0.3457)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'