Diaquabis(1,10-phenanthroline)nickel(II) tetrakis(cyanido-κ<i>C</i>)nickelate(II) tetrahydrofuran solvate monohydrate
Fang, Zhi-li; Wang, Jun; Acta Crystallographica Section E 66 (2010) m1285–; doi:10.1107/S1600536810036974

data_2228166
_publ_section_title
;
 Diaquabis(1,10-phenanthroline)nickel(II)
 tetrakis(cyanido-\k<i>C</i>)nickelate(II) tetrahydrofuran solvate
 monohydrate
;
_journal_coeditor_code           ZL2307
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1285
_journal_paper_doi               10.1107/S1600536810036974
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Ni (C12 H8 N2)2 (H2 O)2] [Ni (C N)4], C4 H8 O, H2 O'
_chemical_formula_moiety
'C24 H20 N4 Ni O2 2+, C4 N4 Ni 2-, C4 H8 O, H2 O'
_chemical_formula_sum            'C32 H30 N8 Ni2 O4'
_chemical_formula_weight         708.06
_chemical_name_systematic
;
Diaquabis(1,10-phenanthroline)nickel(II)
tetrakis(cyanido-\k<i>C</i>)nickelate(II)
tetrahydrofuran solvate monohydrate
;
_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'
_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                 91.189(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4623(3)
_cell_length_b                   14.3184(4)
_cell_length_c                   19.2329(4)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.25
_cell_volume                     3155.86(14)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0983
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29619
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.8071
_exptl_absorpt_correction_T_min  0.7462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6199
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0447P)^2^+1.0970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                3756
_reflns_number_total             6199
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2307.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2228166
_cod_database_fobs_code          2228166