Rhodium(I) Complexes of the Conformationally Rigid IBioxMe4 Ligand: Preparation of Mono-, Bis-, and Tris-ligated NHC Complexes
Chaplin, Adrian B.; Organometallics 33 (2014) 3069–; doi:10.1021/om500332n

data_4089658
_publ_section_title
;
 Rhodium(I) Complexes of the Conformationally Rigid IBioxMe4 Ligand:
 Preparation of Mono-, Bis-, and Tris-ligated NHC Complexes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3069
_journal_paper_doi               10.1021/om500332n
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C33 H48 Cl N6 O6 Rh'
_chemical_formula_sum            'C33 H48 Cl N6 O6 Rh'
_chemical_formula_weight         763.13
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-23
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.11 svn.r2669, GUI svn.r4456)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.135(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5989(4)
_cell_length_b                   17.8176(7)
_cell_length_c                   16.7145(6)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.4796
_cell_measurement_theta_min      2.8859
_cell_volume                     3400.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst (1997), 30, 565.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   25.00  105.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8608   77.0000  120.0000 80

  2 omega   29.00  106.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8608   38.0000 -120.0000 77

  3 omega   -8.00   69.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8608  -99.0000   60.0000 77

  4 omega  -18.00    7.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9546  -99.0000  -90.0000 25

  5 omega  -24.00    1.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9546  -99.0000 -150.0000 25

  6 omega  -63.00   59.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8608  -38.0000  150.0000 122

  7 omega   51.00  113.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8608  159.0000   44.0000 62

  8 omega  -15.00   64.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8608   38.0000    0.0000 79

  9 omega  -25.00   24.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9546  -99.0000   30.0000 49
;
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0297019000
_diffrn_orient_matrix_UB_12      -0.0346922000
_diffrn_orient_matrix_UB_13      -0.0011059000
_diffrn_orient_matrix_UB_21      0.0545633000
_diffrn_orient_matrix_UB_22      0.0187841000
_diffrn_orient_matrix_UB_23      0.0099061000
_diffrn_orient_matrix_UB_31      -0.0009052000
_diffrn_orient_matrix_UB_32      -0.0053461000
_diffrn_orient_matrix_UB_33      0.0419410000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33070
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         3.011
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1592
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2-Heptane at 293 K'
_exptl_crystal_size_max          0.3383
_exptl_crystal_size_mid          0.0989
_exptl_crystal_size_min          0.0492
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 7410 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.941(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         33070
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                27703
_reflns_number_total             33070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500332n_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4089658
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C24(H24A,H24B), C27(H27A,H27B), C39(H39A,H39B),
 C42(H42A,H42B), C9A(H9AA,H9AB), C12A(H12C,H12D), C24A(H24C,H24D), C27A(H27C,
 H27D), C39A(H39C,H39D), C42A(H42C,H42D)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F), C16A(H16D,
 H16E,H16F), C17A(H17D,H17E,H17F), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F),
 C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F), C44A(H44D,H44E,H44F), C45A(H45D,
 H45E,H45F), C46A(H46D,H46E,H46F), C47A(H47D,H47E,H47F)
;