Aqua(dicyanamido){μ-6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}nickel(II)sodium
Wang, Wei; Shen, Yong-Miao; Acta Crystallographica Section E 65 (2009) m557–; doi:10.1107/S160053680901438X

data_2221707
_publ_section_title
Aqua(dicyanamido){\m-6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}nickel(II)sodium
_journal_coeditor_code           HG2500
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m557
_journal_paper_doi               10.1107/S160053680901438X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Na Ni (C18 H18 N2 O4) (C2 N3) (H2 O)]'
_chemical_formula_moiety         'C20 H20 N5 Na Ni O5'
_chemical_formula_sum            'C20 H20 N5 Na Ni O5'
_chemical_formula_weight         492.11
_chemical_name_systematic
;
Aqua(dicyanamido){\m-6,6'-dimethoxy-2,2'-[ethane-1,2-
diylbis(nitrilomethylidyne)]diphenolato}nickel(II)sodium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.282(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4654(14)
_cell_length_b                   22.745(4)
_cell_length_c                   13.177(3)
_cell_measurement_reflns_used    3120
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.568
_cell_measurement_theta_min      2.513
_cell_volume                     2194.2(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10817
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  0.9031
_exptl_absorpt_correction_T_min  0.8790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.352
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3864
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.4335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                2815
_reflns_number_total             3864
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2500.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2221707
_cod_database_fobs_code          2221707