Employing Dianionic Macrocyclic Tetracarbenes To Synthesize Neutral Divalent Metal Complexes
Bass, Heather M.; Cramer, S. Alan; McCullough, Alexander S.; Bernstein, Karl J.; Murdock, Christopher R.; Jenkins, David M.; Organometallics 32 (2013) 2160–; doi:10.1021/om400043z

data_4080508
_publ_section_title
;
 Employing Dianionic Macrocyclic Tetracarbenes To Synthesize Neutral
 Divalent Metal Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2160
_journal_paper_doi               10.1021/om400043z
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C20 H28 B2 N8 Ni'
_chemical_formula_weight         460.83
_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                 126.154(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.058(4)
_cell_length_b                   12.853(3)
_cell_length_c                   11.742(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2200.5(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9586
_diffrn_reflns_theta_full        24.16
_diffrn_reflns_theta_max         24.16
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.9821
_exptl_absorpt_correction_T_min  0.9561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.1054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                1425
_reflns_number_total             1757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400043z_si_002.cif
_cod_data_source_block           Ni
_cod_original_cell_volume        2200.5(11)
_cod_original_sg_symbol_H-M      'c 2/c'
_cod_database_code               4080508