Synthesis and Characterization of a Saddle-Shaped Nickel−Carbene Complex Derived from an Imidazolium-Linkedmeta-Cyclophane
Baker, Murray V.; Skelton, Brian W.; White, Allan H.; Williams, Charlotte C.; Organometallics 21 (2002) 2674–; doi:10.1021/om011031l

data_4076747
_publ_section_title
;
 Synthesis and Characterization of a Saddle-Shaped Nickel&#x2212;Carbene
 Complex Derived from an Imidazolium-Linkedmeta-Cyclophane
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2674
_journal_paper_doi               10.1021/om011031l
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C20 H24 Br2 N6 Ni O3'
_chemical_formula_weight         614.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 94.538(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   7.7950(7)
_cell_length_b                   13.5710(10)
_cell_length_c                   20.789(2)
_cell_measurement_reflns_used    4954
_cell_measurement_temperature    153
_cell_measurement_theta_max      20.1
_cell_measurement_theta_min      2.4
_cell_volume                     2192.3(3)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        xtal
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      153
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .082
_diffrn_reflns_av_sigmaI/netI    .093
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42289
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.567
_exptl_absorpt_correction_T_max  .86
_exptl_absorpt_correction_T_min  .58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       lath
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          .14
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .06
_refine_diff_density_max         1.058
_refine_diff_density_min         -1.318
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_goodness_of_fit_all   1.212
_refine_ls_goodness_of_fit_ref   1.401
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           atomblock
_refine_ls_number_constraints    0
_refine_ls_number_parameters     439
_refine_ls_number_reflns         4068
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .101
_refine_ls_R_factor_gt           .071
_refine_ls_shift/su_max          .048
_refine_ls_shift/su_mean         .01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .09
_refine_ls_wR_factor_ref         .084
_reflns_d_resolution_high        .73
_reflns_d_resolution_low         8.222
_reflns_Friedel_coverage         0
_reflns_limit_h_max              10
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              -28
_reflns_number_gt                4068
_reflns_number_total             5905
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            om011031l.cif
_cod_data_source_block           cw468l
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_original_formula_sum        'C20 H24 Br2 N6 Ni1 O3'
_cod_database_code               4076747