Spiro-fused six-membered N-heterocyclic carbene: a new scaffold toward unique properties and activities
Bin-Miao Yang; Kai Xiang; Yong-Qiang Tu; Shi-Heng Zhang; Deng-Tao Yang; Shao-Hua Wang; Fu-Ming Zhang; Chem.Commun. 50 (2014) 7163–; doi:10.1039/C4CC01627K

data_7114610
_publ_section_title
;
 Spiro-fused six-membered N-heterocyclic carbene: a new scaffold toward
 unique properties and activities
;
_journal_name_full               Chem.Commun.
_journal_page_first              7163
_journal_paper_doi               10.1039/C4CC01627K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C30 H36 Cl N2 Rh'
_chemical_formula_sum            'C30 H36 Cl N2 Rh'
_chemical_formula_weight         562.97
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.161(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1034(3)
_cell_length_b                   19.4323(4)
_cell_length_c                   13.1451(3)
_cell_measurement_reflns_used    5300
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0870
_cell_measurement_theta_min      3.5560
_cell_volume                     2626.73(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics
;
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_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
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.8890
_diffrn_measurement_details
;
  1 omega  -20.00    6.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2137  -99.0000   60.0000 26

  2 omega   -3.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6512   57.0000  120.0000 92

  3 omega   63.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6512   57.0000  150.0000 30

  4 omega   -2.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6512   77.0000  -30.0000 95

  5 omega   42.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6512  -99.0000  120.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0670486000
_diffrn_orient_matrix_UB_12      -0.0063864000
_diffrn_orient_matrix_UB_13      0.0131294000
_diffrn_orient_matrix_UB_21      -0.0114928000
_diffrn_orient_matrix_UB_22      -0.0358947000
_diffrn_orient_matrix_UB_23      0.0004052000
_diffrn_orient_matrix_UB_31      -0.0113394000
_diffrn_orient_matrix_UB_32      -0.0017380000
_diffrn_orient_matrix_UB_33      -0.0567962000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12015
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.037
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             1168
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5352
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0265P)^2^+0.9406P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4367
_reflns_number_total             5352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc01627k2.cif
_cod_data_source_block           yangbm0304
_cod_database_code               7114610
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C23(H23), C26(H26), C27(H27), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C24(H24A,H24B), C25(H25A,H25B), C28(H28A,H28B),
 C29(H29A,H29B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22)
;
_shelx_res_checksum              74601
_shelx_hkl_checksum              79877