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_4088956
_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 Ir2'
_chemical_formula_sum            'C22 H34 Cl4 Ir2'
_chemical_formula_weight         824.69
_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
_audit_creation_date             2016-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.567(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6921(2)
_cell_length_b                   14.9787(4)
_cell_length_c                   11.3445(3)
_cell_measurement_reflns_used    5670
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.1300
_cell_measurement_theta_min      3.8010
_cell_volume                     1231.60(6)
_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      100.00(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
;
  1 omega  -47.00   41.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   57.0000  -60.0000 88

  2 omega  -52.00   38.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   57.0000 -150.0000 90

  3 omega  -94.00   -2.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  133.0000  -50.0000 92

  4 omega -111.00  -85.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  178.0000   90.0000 26

  5 omega  -97.00  -63.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000  150.0000 34

  6 omega -100.00   -7.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000   60.0000 93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0004537000
_diffrn_orient_matrix_UB_12      0.0471658000
_diffrn_orient_matrix_UB_13      -0.0060348000
_diffrn_orient_matrix_UB_21      0.0321988000
_diffrn_orient_matrix_UB_22      0.0043694000
_diffrn_orient_matrix_UB_23      0.0660668000
_diffrn_orient_matrix_UB_31      0.0923307000
_diffrn_orient_matrix_UB_32      -0.0017235000
_diffrn_orient_matrix_UB_33      0.0005072000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12108
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        30.500
_diffrn_reflns_theta_max         32.394
_diffrn_reflns_theta_min         3.812
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.235
_exptl_absorpt_correction_T_max  0.591
_exptl_absorpt_correction_T_min  0.189
_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    2.224
_exptl_crystal_description       rod
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.4545
_exptl_crystal_size_mid          0.0873
_exptl_crystal_size_min          0.0738
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         4076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0001P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3492
_reflns_number_total             4076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           2a_lbx1-011abs
_cod_original_cell_volume        1231.60(7)
_cod_database_code               4088956
_chemical_oxdiff_formula         'C22 H34 Cl4 Ir2'
_chemical_oxdiff_usercomment     ERI19
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.03) H6B(0.03) H6C(0.03) H7A(0.035) H7B(0.035) H7C(0.035)
 H8A(0.039) H8B(0.039) H8C(0.039) H9A(0.034) H9B(0.034) H9C(0.034) H10A(0.017)
 H10B(0.017) H11A(0.033) H11B(0.033) H11C(0.033)
 Fixed X: H6A(0.5566) H6B(0.4044) H6C(0.535) H7A(0.4012) H7B(0.1845) H7C(0.3)
 H8A(0.0641) H8B(-0.1122) H8C(-0.0434) H9A(-0.0295) H9B(-0.1139) H9C(0.068)
 H10A(0.4135) H10B(0.2768) H11A(0.1603) H11B(0.175) H11C(0.0229)
 Fixed Y: H6A(0.4518) H6B(0.4066) H6C(0.3455) H7A(0.2325) H7B(0.2122)
 H7C(0.2082) H8A(0.2622) H8B(0.2956) H8C(0.3504) H9A(0.505) H9B(0.5425)
 H9C(0.5867) H10A(0.5857) H10B(0.6256) H11A(0.5669) H11B(0.6693) H11C(0.6059)
 Fixed Z: H6A(0.1335) H6B(0.016) H6C(0.1258) H7A(0.1853) H7B(0.1371)
 H7C(0.2834) H8A(0.3658) H8B(0.2532) H8C(0.3817) H9A(0.3709) H9B(0.2312)
 H9C(0.327) H10A(0.1621) H10B(0.2288) H11A(-0.027) H11B(0.0155) H11C(0.0396)
;
_shelx_res_checksum              67610
_shelx_hkl_checksum              80054
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'