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_4337278
_publ_section_title
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 Synthesis, structural characterization, and magnetic properties of a
 copper-gadolinium complex derived from a hydroxybenzohydrazide ligand.
;
_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 unk
_chemical_formula_moiety         'C20 H23 Cu N3 O4, 0.5(H2 O)'
_chemical_formula_sum            'C20 H24 Cu N3 O4.5'
_chemical_formula_weight         441.97
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 107.783(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3862(4)
_cell_length_b                   19.1051(7)
_cell_length_c                   18.6796(7)
_cell_measurement_reflns_used    9507
_cell_measurement_temperature    100
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     3869.3(2)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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  '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  0.034
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            91884
_diffrn_reflns_theta_full        29.033
_diffrn_reflns_theta_max         29.033
_diffrn_reflns_theta_min         2.132
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.10
_refine_diff_density_min         -0.41
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0400
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         16585
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.0016026
_refine_ls_shift/su_mean         0.0000300
_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: 
 0.250 0.286 0.157 0.574E-01 0.121E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0387
_refine_ls_wR_factor_gt          0.0329
_refine_ls_wR_factor_ref         0.0319
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              -25
_reflns_number_gt                17342
_reflns_number_total             18806
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0279
_oxford_reflns_number_all        18742
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic4027283_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_Hall     'P -2yac '
_cod_original_sg_symbol_H-M      'P n '
_cod_original_formula_sum        'C20 H24 Cu1 N3 O4.50'
_cod_database_code               4337278
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
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   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
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RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 201,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) 
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RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) H   (1153,X'S) H   (1152,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) H   (1162,X'S) 
RIDE C   ( 117,X'S) H   (1172,X'S) H   (1171,X'S) 
RIDE C   ( 118,X'S) H   (1182,X'S) H   (1181,X'S) 
RIDE C   ( 119,X'S) H   (1191,X'S) H   (1192,X'S) 
RIDE C   ( 120,X'S) H   (1202,X'S) H   (1201,X'S) 
RIDE C   ( 203,X'S) H   (2031,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) 
RIDE C   ( 205,X'S) H   (2051,X'S) 
RIDE C   ( 207,X'S) H   (2071,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) 
RIDE C   ( 213,X'S) H   (2131,X'S) 
RIDE C   ( 215,X'S) H   (2151,X'S) H   (2153,X'S) H   (2152,X'S) 
RIDE C   ( 216,X'S) H   (2161,X'S) H   (2162,X'S) 
RIDE C   ( 217,X'S) H   (2172,X'S) H   (2171,X'S) 
RIDE C   ( 218,X'S) H   (2182,X'S) H   (2181,X'S) 
RIDE C   ( 219,X'S) H   (2191,X'S) H   (2192,X'S) 
RIDE C   ( 220,X'S) H   (2202,X'S) H   (2201,X'S) 
RIDE C   ( 303,X'S) H   (3031,X'S) 
RIDE C   ( 304,X'S) H   (3041,X'S) 
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RIDE C   ( 307,X'S) H   (3071,X'S) 
RIDE C   ( 310,X'S) H   (3101,X'S) 
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RIDE C   ( 316,X'S) H   (3161,X'S) H   (3162,X'S) 
RIDE C   ( 317,X'S) H   (3172,X'S) H   (3171,X'S) 
RIDE C   ( 318,X'S) H   (3182,X'S) H   (3181,X'S) 
RIDE C   ( 319,X'S) H   (3191,X'S) H   (3192,X'S) 
RIDE C   ( 320,X'S) H   (3202,X'S) H   (3201,X'S) 
RIDE N   (  3,X'S) H   ( 32,X'S) 
RIDE N   ( 103,X'S) H   (1032,X'S) 
RIDE N   ( 203,X'S) H   (2032,X'S) 
RIDE N   ( 303,X'S) H   (3032,X'S) 
RIDE O   (  4,X'S) H   ( 42,X'S) 
RIDE O   (  5,X'S) H   ( 52,X'S) H   ( 53,X'S) 
RIDE O   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE O   ( 104,X'S) H   (1042,X'S) 
RIDE O   ( 204,X'S) H   (2042,X'S) 
RIDE O   ( 304,X'S) H   (3042,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
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