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_4334055
_publ_contact_author_address
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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
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 Heptacoordinated Nickel(II) as an Ising-Type Anisotropic Building Unit:
 Illustration with a Pentanuclear [(NiL)3{W(CN)8}2] Complex
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_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_absolute_configuration ad
_chemical_formula_moiety         'C121 H91 N31 Ni3 O8 W2'
_chemical_formula_sum            'C121 H91 N31 Ni3 O8 W2'
_chemical_formula_weight         2651.10
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 98.685(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0517(4)
_cell_length_b                   30.9780(11)
_cell_length_c                   21.1989(7)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     7174.4(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.044
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            88535
_diffrn_reflns_theta_full        25.203
_diffrn_reflns_theta_max         26.253
_diffrn_reflns_theta_min         1.173
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.041
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         2.29
_refine_diff_density_min         -2.76
_refine_ls_abs_structure_details 'Flack (1983), 12338 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.139(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1499
_refine_ls_number_reflns         23252
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.0062841
_refine_ls_shift/su_mean         0.0001000
_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: 
 0.512 0.289 0.354 0.818E-01 0.435E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0566
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0528
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              38
_reflns_limit_k_min              -37
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                24685
_reflns_number_total             26677
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0532
_oxford_reflns_number_all        26560
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic3027368_si_004.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               4334055
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C(82,U'S) C(820, U'S) 
RIDE C(83,U'S) C(830, U'S) 
RIDE C(85,U'S) C(850, U'S) 
RIDE C(86,U'S) C(860, U'S) 
RIDE O(3,X'S) H(31,X'S) H(32,X'S) 
RIDE O(8,X'S) H(81,X'S) H(82,X'S) 
RIDE N(19,X'S) H(19,X'S) 
RIDE N(20,X'S) H(20,X'S) 
RIDE N(24,X'S) H(24,X'S) 
RIDE N(25,X'S) H(25,X'S) 
RIDE N(29,X'S) H(29,X'S) 
RIDE N(30,X'S) H(30,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  27,X'S) H   ( 273,X'S) H   ( 272,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   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) H   ( 583,X'S) 
RIDE C   (  62,X'S) H   ( 623,X'S) H   ( 622,X'S) H   ( 621,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) H   ( 932,X'S) H   ( 933,X'S) 
RIDE C   (  97,X'S) H   ( 971,X'S) H   ( 972,X'S) H   ( 973,X'S) 
RIDE C   (  99,X'S) H   ( 991,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 119,X'S) H   (1191,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) 
RIDE C   ( 121,X'S) H   (1211,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
SAME C(81) C(82) C(83) C(84) C(85) C(86) AND 
CONT C(81) C(820) C(830) C(84) C(850) C(860) 
DELU 0.01 C(82) C(83) C(85) C(86) AND 
CONT C(820) C(830)C(850) C(860) 
SIMU 0.01 C(82) C(83) C(85) C(86) AND 
CONT C(820) C(830)C(850) C(860) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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