Synthesis and Crystal Structures of Binuclear Metallocyclophane with N-Heterocyclic Carbene Linkage by the π−π Stacking Interaction
Wan, Xiang-Jian; Xu, Feng-Bo; Li, Qing-Shan; Song, Hai-Bin; Zhang, Zheng-Zhi; Organometallics 24 (2005) 6066–; doi:10.1021/om050443h

data_4076018
_publ_section_title
;
 Synthesis and Crystal Structures of Binuclear Metallocyclophane with
 N-Heterocyclic Carbene Linkage by the \p&#x2212;\p Stacking Interaction
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6066
_journal_paper_doi               10.1021/om050443h
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C17.5 H20.25 F6 Hg0.5 N3.75 O P'
_chemical_formula_weight         544.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 126.142(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   21.634(3)
_cell_length_b                   34.632(5)
_cell_length_c                   14.4450(19)
_cell_measurement_reflns_used    4093
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.61
_cell_volume                     8740(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25327
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    3.687
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.807153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4296
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.991
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         8945
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+9.7218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                5849
_reflns_number_total             8945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050443hsi20050602_111744.cif
_cod_data_source_block           complex_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        8739.8(19)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C17.50 H20.25 F6 Hg0.50 N3.75 O P'
_cod_database_code               4076018