Synthesis, structural characterization, and magnetic properties of a copper-gadolinium complex derived from a hydroxybenzohydrazide ligand.
Costes, Jean-Pierre; Duhayon, Carine; Vendier, Laure; Inorganic chemistry 53 (2014) 2181–2187; doi:10.1021/ic4027283

data_4337279
_publ_section_title
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 Synthesis, structural characterization, and magnetic properties of a
 copper-gadolinium complex derived from a hydroxybenzohydrazide ligand.
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_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2181
_journal_page_last               2187
_journal_paper_doi               10.1021/ic4027283
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C60 H48 Cu4 N8 O16'
_chemical_formula_sum            'C60 H48 Cu4 N8 O16'
_chemical_formula_weight         1391.27
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.8827(3)
_cell_length_b                   16.8827(3)
_cell_length_c                   12.6346(2)
_cell_measurement_reflns_used    13374
_cell_measurement_temperature    100
_cell_measurement_theta_max      61
_cell_measurement_theta_min      4
_cell_volume                     3601.18(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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.038
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27154
_diffrn_reflns_theta_full        60.602
_diffrn_reflns_theta_max         60.602
_diffrn_reflns_theta_min         3.498
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.863
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.44
_refine_ls_abs_structure_details 'Flack (1983), 2557 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4856
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.0005241
_refine_ls_shift/su_mean         0.0000228
_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: 
 19.3 7.36 16.1 3.31 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0915
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0853
_reflns_limit_h_max              19
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                5028
_reflns_number_total             5425
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0735
_oxford_reflns_number_all        5395
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic4027283_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        3601.20(10)
_cod_original_sg_symbol_Hall     'P -4 '
_cod_original_sg_symbol_H-M      'P -4 '
_cod_database_code               4337279
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
GROUP  C(9) C(10) C(11) C(12) C(13) C(14) 
GROUP C(90) C(100) C(110) C(120) C(130) C(140) 
RIDE C(8,U'S) C(9,U'S) C(90,U'S) C(10,U'S) C(100,U'S) 
CONT C(11,U'S) C(110,U'S) C(12,U'S) C(120,U'S) 
CONT C(13,U'S) C(130,U'S) C(14,U'S) C(140,U'S) 
CONT O(4,U'S) O(40,U'S) 
GROUP  C(29) C(30) C(31) C(32) C(33) C(34) 
GROUP C(290) C(300) C(310) C(320) C(330) C(340) 
RIDE C(29,U'S) C(290,U'S) C(30,U'S) C(300,U'S) 
CONT C(31,U'S) C(310,U'S) 
CONT C(32,U'S) C(320,U'S) C(33,U'S) C(330,U'S) 
CONT C(34,U'S) C(340,U'S) O(24,U'S) O(240,U'S) 
RIDE O(2,U'S) O(20,U'S) C(15,U'S) C(150,U'S) 
RIDE O(22,U'S) O(220,U'S) C(35,U'S) C(350,U'S) 
RIDE O(2,X'S) O(20,X'S) C(15,X'S) C(150,X'S) 
RIDE O(22,X'S) O(220,X'S) C(35,X'S) C(350,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,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   (  27,X'S) H   ( 271,X'S) 
RIDE O   (  4,X'S) H   ( 4,X'S) 
RIDE O   (  24,X'S) H   ( 24,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
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