[7,16-Bis(benzyloxycarbonyl)-6,18,15,17-tetramethyldibenzo[<i>b</i>,<i>i</i>][1,4,8,11]tetraazacyclotetradecinato-κ^4^<i>N</i>]nickel(II)
Boyd, Peter D.W.; Challis, J.B.; Rickard, C.E.F.; Acta Crystallographica Section E 62 (2006) m2732–m2734; doi:10.1107/S1600536806038803

data_2210733
_publ_section_title
'[7,16-Bis(benzyloxycarbonyl)-6,18,15,17-tetramethyldibenzo[<i>b</i>,<i>i</i>][1,4,8,11]tetraazacyclotetradecinato-\k^4^<i>N</i>]nickel(II)'
_journal_coeditor_code           NG2105
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2732
_journal_page_last               m2734
_journal_paper_doi               10.1107/S1600536806038803
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ni (C38 H34 N4 O4)]'
_chemical_formula_moiety         'C38 H34 N4 Ni O4'
_chemical_formula_sum            'C38 H34 N4 Ni O4'
_chemical_formula_weight         669.40
_chemical_name_systematic
;
[7,16-Bis(benzyloxycarbonyl)-6,18,15,17-
tetramethyldibenzo[b,i][1,4,8,11]tetraazacyclotetradecinato-\k^4^N]nickel(II)
;
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.6079(2)
_cell_length_b                   40.5916(2)
_cell_length_c                   14.8774(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      1
_cell_volume                     6406.08(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33114
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        <2%
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.9026
_exptl_absorpt_correction_T_min  0.7986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.847
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.847
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+14.0271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                4985
_reflns_number_total             5855
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2105.cif
_cod_data_source_block           I
_cod_database_code               2210733
_cod_database_fobs_code          2210733