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_4089659
_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         'C13 H16 Cl N2 O4 Rh'
_chemical_formula_sum            'C13 H16 Cl N2 O4 Rh'
_chemical_formula_weight         402.64
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-26
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.332(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3855(16)
_cell_length_b                   9.5589(6)
_cell_length_c                   12.9231(8)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.6243
_cell_measurement_theta_min      2.8109
_cell_volume                     3122.3(3)
_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
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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   -1.00  107.00   1.0000    3.1400
omega____ theta____ kappa____ phi______ frames
    -       17.3347    0.0000   60.0000 108

  2 omega  -38.00  -12.00   1.0000    3.1400
omega____ theta____ kappa____ phi______ frames
    -       17.3347    0.0000   60.0000 26

  3 omega  -28.00   56.00   1.0000    3.1400
omega____ theta____ kappa____ phi______ frames
    -       17.3347   19.0000 -180.0000 84

  4 omega -104.00  -77.00   1.0000    3.1400
omega____ theta____ kappa____ phi______ frames
    -      -18.2722 -178.0000  -90.0000 27

  5 omega   -9.00   93.00   1.0000    3.1400
omega____ theta____ kappa____ phi______ frames
    -       17.3347   38.0000 -120.0000 102

  6 omega  -25.00   59.00   1.0000    3.1400
omega____ theta____ kappa____ phi______ frames
    -       17.3347  -99.0000   90.0000 84

  7 omega  -25.00   22.00   1.0000    3.1400
omega____ theta____ kappa____ phi______ frames
    -      -18.2722  -99.0000  -90.0000 47

  8 omega -108.00  -57.00   1.0000    3.1400
omega____ theta____ kappa____ phi______ frames
    -      -18.2722 -178.0000 -180.0000 51
;
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0097097000
_diffrn_orient_matrix_UB_12      -0.0587036000
_diffrn_orient_matrix_UB_13      0.0259576000
_diffrn_orient_matrix_UB_21      0.0261701000
_diffrn_orient_matrix_UB_22      -0.0179352000
_diffrn_orient_matrix_UB_23      0.0191437000
_diffrn_orient_matrix_UB_31      -0.0024317000
_diffrn_orient_matrix_UB_32      0.0417585000
_diffrn_orient_matrix_UB_33      0.0447189000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22242
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.572
_diffrn_reflns_theta_max         29.572
_diffrn_reflns_theta_min         3.166
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89836
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_recrystallization_method
'Crystals grown from Benzene-Heptane at 278 K'
_exptl_crystal_size_max          0.4000
_exptl_crystal_size_mid          0.3000
_exptl_crystal_size_min          0.0800
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0216P)^2^+3.2208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3750
_reflns_number_total             4373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500332n_si_002.cif
_cod_data_source_block           4
_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               4089659
_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:
 C13(H13A,H13B), C16(H16A,H16B)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C)
;