Di-μ-cyanido-tetracyanido(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)[<i>N</i>-(quinolin-8-yl)quinoline-2-carboxamidato]diiron(III)nickel(II) 2.07-hydrate
Yang, Yuqi; Zhou, Hongbo; Shen, Xiaoping; Acta Crystallographica Section E 69 (2013) m271–m272; doi:10.1107/S1600536813010234

data_2238108
_publ_section_title
;
 Di-\m-cyanido-tetracyanido(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)[<i>N</i>-(quinolin-8-yl)quinoline-2-carboxamidato]diiron(III)nickel(II)
 2.07-hydrate
;
_journal_coeditor_code           ZL2544
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m271
_journal_page_last               m272
_journal_paper_doi               10.1107/S1600536813010234
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
'[Fe2 Ni (C19 H12 N3 O)2 (C N)6 (C16 H36 N4)], 2.07H2 O'
_chemical_formula_moiety         'C60 H60 Fe2 N16 Ni O2, 2.07(H2 O)'
_chemical_formula_sum            'C60 H64.14 Fe2 N16 Ni O4.07'
_chemical_formula_weight         1244.89
_chemical_name_systematic
'Di-\m-cyanido-tetracyanido(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)[<i>N</i>-(quinolin-8-yl)quinoline-2-carboxamidato]diiron(III)nickel(II) dihydrate'
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.781(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4145(13)
_cell_length_b                   15.7309(17)
_cell_length_c                   20.590(2)
_cell_measurement_reflns_used    3735
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      23.42
_cell_measurement_theta_min      2.11
_cell_volume                     2985.1(6)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rigaku Saturn 724 CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12764
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.8346
_exptl_absorpt_correction_T_min  0.7963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1297.4
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.420
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         5722
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0950P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                4078
_reflns_number_total             5722
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2544.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238108
_cod_database_fobs_code          2238108