Synthesis, Crystal Structure, and Properties of a 3-D Network Assembled by Nickel(II) Macrocyclic Complex and Terephthalato Bridge
Hye Jin Choi; Myunghyun Paik Suh; Inorganic Chemistry 38 (1999) 6309–6312; doi:10.1021/ic990664d

data_4322550
_publ_section_title
;
 Synthesis, Crystal Structure, and Properties of a 3-D Network Assembled
 by Nickel(II) Macrocyclic Complex and Terephthalato Bridge
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6309
_journal_page_last               6312
_journal_paper_doi               10.1021/ic990664d
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C10 H21 N3 Ni0.5 O5'
_chemical_formula_weight         292.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 121.637(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.182(2)
_cell_length_b                   9.035(2)
_cell_length_c                   16.431(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2677.2(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0107
_diffrn_reflns_av_sigmaI/netI    0.1318
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5001
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.787
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_F_000             1248
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.0002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.883
_refine_ls_goodness_of_fit_obs   1.227
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         4710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.883
_refine_ls_restrained_S_obs      1.227
_refine_ls_R_factor_all          0.1819
_refine_ls_R_factor_obs          0.0486
_refine_ls_shift/esd_max         0.864
_refine_ls_shift/esd_mean        0.159
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1599
_refine_ls_wR_factor_obs         0.1045
_reflns_number_observed          1305
_reflns_number_total             4710
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990664d.cif
_cod_data_source_block           xtal
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2677.3(7)
_cod_original_formula_sum        'C10 H21 N3 Ni0.50 O5'
_cod_database_code               4322550