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_4088972
_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         'C30 H46 Cl4 Rh2'
_chemical_formula_sum            'C30 H46 Cl4 Rh2'
_chemical_formula_weight         754.29
_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             2015-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.806(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6334(3)
_cell_length_b                   19.1231(4)
_cell_length_c                   8.7620(2)
_cell_measurement_reflns_used    16937
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.3460
_cell_measurement_theta_min      4.1170
_cell_volume                     1696.35(8)
_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)'
_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 0.954
_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   -104.00  45.00   1.00   18.00    --  -29.53   0.00 150.00  149
  2  \w   -102.00   4.00   1.00   18.00    --  -29.53 -77.00 -30.00  106
  3  \w    -63.00  43.00   1.00   18.00    --  -29.53  77.00-180.00  106
  4  \w    -63.00  43.00   1.00   18.00    --  -29.53  77.00  90.00  106
  5  \w    -63.00  43.00   1.00   18.00    --  -29.53  77.00 -90.00  106
  6  \w   -102.00   4.00   1.00   18.00    --  -29.53 -77.00-150.00  106
  7  \w   -109.00 -35.00   1.00   18.00    --  -29.53-178.00-120.00   74
  8  \w   -100.00  -6.00   1.00   18.00    --  -29.53 -57.00  30.00   94
  9  \w   -102.00   4.00   1.00   18.00    --  -29.53 -77.00 150.00  106
 10  \w   -100.00  -6.00   1.00   18.00    --  -29.53 -57.00  90.00   94
 11  \w   -100.00 -75.00   1.00   18.00    --  -29.53 -57.00-120.00   25
;
_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      0.0673461000
_diffrn_orient_matrix_UB_12      0.0223222000
_diffrn_orient_matrix_UB_13      0.0101900000
_diffrn_orient_matrix_UB_21      -0.0190543000
_diffrn_orient_matrix_UB_22      0.0049111000
_diffrn_orient_matrix_UB_23      -0.0692209000
_diffrn_orient_matrix_UB_31      -0.0482159000
_diffrn_orient_matrix_UB_32      0.0292043000
_diffrn_orient_matrix_UB_33      0.0039408000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            43435
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        31.000
_diffrn_reflns_theta_max         32.439
_diffrn_reflns_theta_min         3.763
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.696
_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    1.477
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         5826
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0257P)^2^+2.0693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5088
_reflns_number_total             5826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00580_si_002.cif
_cod_data_source_block           3n_lbx-034
_cod_original_cell_volume        1696.35(7)
_cod_database_code               4088972
_chemical_oxdiff_formula         'C30 H46 Cl4 Rh2 C H2 Cl2'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.023) H7A(0.064) H7B(0.064) H8A(0.086) H8B(0.086) H9A(0.094)
 H9B(0.094) H10A(0.088) H10B(0.088) H11A(0.088) H11B(0.088) H6B(0.021)
 H7C(0.03) H7D(0.03) H8C(0.038) H8D(0.038) H9C(0.042) H9D(0.042) H10C(0.021)
 H10D(0.021) H11C(0.039) H11D(0.039) H12A(0.035) H12B(0.035) H12C(0.035)
 H13A(0.033) H13B(0.033) H13C(0.033) H14A(0.038) H14B(0.038) H14C(0.038)
 H15A(0.041) H15B(0.041) H15C(0.041)
 Fixed X: H6A(0.8503) H7A(0.8786) H7B(0.9109) H8A(1.0728) H8B(1.1153)
 H9A(1.1266) H9B(1.2171) H10A(1.0519) H10B(1.0875) H11A(0.9004) H11B(0.8542)
 H6B(0.8637) H7C(0.9065) H7D(0.8676) H8C(1.0732) H8D(1.0987) H9C(1.0879)
 H9D(1.1277) H10C(1.1399) H10D(1.2269) H11C(0.8937) H11D(0.9246) H12A(0.7179)
 H12B(0.7131) H12C(0.5843) H13A(0.3756) H13B(0.3789) H13C(0.2903) H14A(0.2874)
 H14B(0.3747) H14C(0.3682) H15A(0.5892) H15B(0.6518) H15C(0.7415)
 Fixed Y: H6A(0.4311) H7A(0.3542) H7B(0.291) H8A(0.4137) H8B(0.3352)
 H9A(0.3045) H9B(0.3722) H10A(0.443) H10B(0.3848) H11A(0.3176) H11B(0.3942)
 H6B(0.3418) H7C(0.2997) H7D(0.2486) H8C(0.2636) H8D(0.2436) H9C(0.403)
 H9D(0.451) H10C(0.3535) H10D(0.3355) H11C(0.4554) H11D(0.4294) H12A(0.2711)
 H12B(0.2162) H12C(0.2295) H13A(0.2622) H13B(0.2274) H13C(0.2953) H14A(0.3829)
 H14B(0.3846) H14C(0.452) H15A(0.499) H15B(0.4446) H15C(0.4776)
 Fixed Z: H6A(0.4503) H7A(0.255) H7B(0.3814) H8A(0.3978) H8B(0.3724)
 H9A(0.6445) H9B(0.6528) H10A(0.6798) H10B(0.818) H11A(0.673) H11B(0.708)
 H6B(0.6128) H7C(0.3217) H7D(0.4443) H8C(0.6358) H8D(0.4701) H9C(0.7096)
 H9D(0.5814) H10C(0.4231) H10D(0.6021) H11C(0.5451) H11D(0.3867) H12A(0.6689)
 H12B(0.5294) H12C(0.5836) H13A(0.4558) H13B(0.2909) H13C(0.2884) H14A(0.1208)
 H14B(0.0009) H14C(0.1064) H15A(0.1725) H15B(0.0773) H15C(0.2427)
;
_shelx_res_checksum              70104
_shelx_hkl_checksum              87809
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-10-20
_olex2_date_sample_submission    2015-10-20
_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 1.131
_oxdiff_exptl_absorpt_empirical_full_min 0.883