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_4089661
_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         'C23 H32 Cl N4 O5 Rh'
_chemical_formula_sum            'C23 H32 Cl N4 O5 Rh'
_chemical_formula_weight         582.88
_chemical_melting_point          ?
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-27
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.03.22 svn.r2654, GUI svn.r4446)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.6132(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.23498(17)
_cell_length_b                   11.4086(2)
_cell_length_c                   10.78784(18)
_cell_measurement_reflns_used    9595
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3912
_cell_measurement_theta_min      2.9996
_cell_volume                     1241.97(4)
_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  -15.00  104.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -       21.8608   38.0000   30.0000 119

  2 omega -112.00  -83.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      -22.7983 -178.0000  -90.0000 29

  3 omega  -24.00   22.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      -22.7983  -99.0000  150.0000 46

  4 omega  -41.00   17.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      -22.7983  -19.0000  150.0000 58

  5 omega  -63.00   59.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -       21.8608  -38.0000  -90.0000 122

  6 omega  -63.00   59.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -       21.8608  -38.0000   30.0000 122

  7 omega  -25.00   22.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      -22.7983  -99.0000   30.0000 47

  8 omega -117.00  -53.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      -22.7983  178.0000   90.0000 64
;
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0464990000
_diffrn_orient_matrix_UB_12      -0.0440167000
_diffrn_orient_matrix_UB_13      0.0089125000
_diffrn_orient_matrix_UB_21      -0.0506073000
_diffrn_orient_matrix_UB_22      0.0430217000
_diffrn_orient_matrix_UB_23      -0.0045597000
_diffrn_orient_matrix_UB_31      -0.0146538000
_diffrn_orient_matrix_UB_32      -0.0089281000
_diffrn_orient_matrix_UB_33      -0.0659245000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17744
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.573
_diffrn_reflns_theta_max         29.573
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95957
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2-Heptane at 293 K'
_exptl_crystal_size_max          0.3800
_exptl_crystal_size_mid          0.2500
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+1.0847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2993
_reflns_number_total             3483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500332n_si_002.cif
_cod_data_source_block           7
_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               4089661
_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. Others
 Fixed Sof: Cl2(0.5) O4(0.5) C3(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C14(H14A,H14B)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C)
;