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_4334054
_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
'C85 H67 N31 Ni3 O8 W2, 0.667(C2 H3 N), 12(H2 O)'
_chemical_formula_sum            'C86.33 H93 N31.67 Ni3 O20 W2'
_chemical_formula_weight         2438.02
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 90.1820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.1095(2)
_cell_length_b                   16.87280(10)
_cell_length_c                   21.41700(10)
_cell_measurement_reflns_used    77635
_cell_measurement_temperature    180
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     10519.09(11)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (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 0.963
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            268892
_diffrn_reflns_theta_full        28.189
_diffrn_reflns_theta_max         30.640
_diffrn_reflns_theta_min         3.375
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.785
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       stick
_exptl_crystal_F_000             4898.608
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.11
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0314
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         12257
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.0024868
_refine_ls_shift/su_mean         0.0000509
_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: 
 18.1 12.3 15.5 8.08 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0549
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0391
_reflns_limit_h_max              41
_reflns_limit_h_min              -41
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                12919
_reflns_number_total             15634
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0319
_oxford_reflns_number_all        15613
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic3027368_si_003.cif
_cod_data_source_block           1
_cod_original_cell_volume        10519.10(11)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4334054
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE W(1,X'S, U'S) UNTIL O(10) C(9,X'S,U[ISO]) UNTIL N(9) 
RIDE C(9,U[ISO]) C(10,U[ISO]) N(9,U[ISO]) 
RIDE O   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE N   (  13,X'S) H   ( 131,X'S) 
RIDE N   (  14,X'S) H   ( 141,X'S) 
RIDE N   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 452,X'S) 
RIDE C   (  14,X'S) H   ( 453,X'S) 
RIDE C   (  17,X'S) H   ( 173,X'S) H   ( 172,X'S) H   ( 171,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  38,X'S) H   ( 383,X'S) H   ( 382,X'S) H   ( 381,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE O   (   5,X'S) H   (  51,X'S) H   (  52,X'S) 
RIDE O   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE O   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE O   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C (9,X'S) H(93,X'S) H(94,X'S) H(95,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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