Heptacoordinated Nickel(II) as an Ising-Type Anisotropic Building Unit: Illustration with a Pentanuclear [(NiL)3{W(CN)8}2] Complex
Nayanmoni Gogoi; Mehrez Thlijeni; Carine Duhayon; Jean-Pascal Sutter; Inorganic Chemistry 52 (2013) 2283–2285; doi:10.1021/ic3027368

data_4334053
_publ_contact_author_address
; 
Laboratoire de Chimie de Coordination du CNRS
205, route de Narbonne
31077 Toulouse (France)
;
_publ_contact_author_email       sutter@lcc-toulouse.fr
_publ_contact_author_fax         '(33) 5 61 55 30 03'
_publ_contact_author_name        'Jean-Pascal Sutter'
_publ_contact_author_phone       '(33) 5 61 33 31 57 '
_publ_section_title
;
 Heptacoordinated Nickel(II) as an Ising-Type Anisotropic Building Unit:
 Illustration with a Pentanuclear [(NiL)3{W(CN)8}2] Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2283
_journal_page_last               2285
_journal_paper_doi               10.1021/ic3027368
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C36 H33 N6 Ni O6, 0.5(C H4 O), N O3'
_chemical_formula_sum            'C36.5 H35 N7 Ni O9.5'
_chemical_formula_weight         782.43
_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
_cell_angle_alpha                90
_cell_angle_beta                 97.8721(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.39928(16)
_cell_length_b                   18.0571(3)
_cell_length_c                   23.6812(3)
_cell_measurement_reflns_used    17087
_cell_measurement_temperature    180
_cell_measurement_theta_max      71
_cell_measurement_theta_min      3
_cell_volume                     3557.80(10)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35442
_diffrn_reflns_theta_full        69.321
_diffrn_reflns_theta_max         70.735
_diffrn_reflns_theta_min         3.088
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             1626
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.74
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         5951
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.0015131
_refine_ls_shift/su_mean         0.0000424
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 18.5 15.5 15.7 5.43 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0853
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0824
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                6171
_reflns_number_total             6779
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0717
_oxford_reflns_number_all        6750
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic3027368_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C36.50 H35 N7 Ni1 O9.50'
_cod_database_code               4334053