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_4337280
_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_formula_moiety         'C74 H108 Cu2 Gd2 N4 O18'
_chemical_formula_sum            'C74 H108 Cu2 Gd2 N4 O18'
_chemical_formula_weight         1775.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 112.462(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8730(11)
_cell_length_b                   17.923(3)
_cell_length_c                   26.0370(15)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    180
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     9001.6(17)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_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      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_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  0.115
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18371
_diffrn_reflns_theta_full        26.375
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_min         3.162
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.979
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
;
_refine_diff_density_max         2.13
_refine_diff_density_min         -1.39
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1365
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         6940
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.0069730
_refine_ls_shift/su_mean         0.0001383
_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: 
 9.55 -4.09 6.42 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1062
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0694
_reflns_limit_h_max              24
_reflns_limit_h_min              -26
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                8488
_reflns_number_total             18371
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0603
_oxford_reflns_number_all        18345
_oxford_reflns_threshold_expression_ref I>2.8\s(I)
_cod_data_source_file            ic4027283_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4337280
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, U'S 
RIDE C(50,U'S) C(51,U'S) C(52,U'S) 
CONT C(500,U'S) C(510,U'S) C(520,U'S) 
RIDE C(65,U'S) C(66,U'S) C(67,U'S) 
CONT C(650,U'S) C(660,U'S) C(670,U'S) 
RIDE C(34,U'S) C(42,U'S) C(43,U'S) 
RIDE C(39,U'S) C(40,U'S) C(41,U'S) 
RIDE C(61,U'S) C(62,U'S) C(63,U'S) 
RIDE O   (   9,X'S) H   (  1,X'S) 
RIDE O   (   10,X'S) H   (  2,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) 
RIDE C   (  15,X'S) H   ( 152,X'S) H   ( 153,X'S) H   ( 151,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   (  22,X'S) H   ( 221,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   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 303,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 333,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 343,X'S) H   ( 342,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) H   ( 393,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 433,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) H   ( 443,X'S) 
RIDE C   (  45,X'S) H   ( 453,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 543,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 552,X'S) H   ( 551,X'S) H   ( 553,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 563,X'S) H   ( 562,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) H   ( 612,X'S) H   ( 613,X'S) 
RIDE C   (  62,X'S) H   ( 622,X'S) H   ( 623,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,X'S) H   ( 633,X'S) 
RIDE C   (  65,X'S) H   ( 652,X'S) H   ( 653,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 663,X'S) H   ( 662,X'S) 
RIDE C   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) H   ( 673,X'S) 
RIDE C   (  650,X'S) H   ( 6502,X'S) H   ( 6503,X'S) H   ( 6501,X'S) 
RIDE C   (  660,X'S) H   ( 6601,X'S) H   ( 6603,X'S) H   ( 6602,X'S) 
RIDE C   (  670,X'S) H   ( 6702,X'S) H   ( 6701,X'S) H   ( 6703,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  72,X'S) H   ( 723,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) H   ( 733,X'S) 
RIDE C   (  74,X'S) H   ( 742,X'S) H   ( 743,X'S) H   ( 741,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) H   ( 523,X'S) 
RIDE C   ( 520,X'S) H   (5201,X'S) H   (5202,X'S) H   (5203,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) H   ( 503,X'S) 
RIDE C   ( 500,X'S) H   (5001,X'S) H   (5002,X'S) H   (5003,X'S) 
RIDE C   ( 510,X'S) H   (5101,X'S) H   (5102,X'S) H   (5103,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) H   ( 513,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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DIST 1.54,0.02=C(48) TO C(49) 
CONT C(49) TO C(50), C(49) TO C(51), C(49) TO C(52) 
CONT C(49) TO C(500), C(49) TO C(510), C(49) TO C(520) 
SAME C(49) C(50) C(51) C(52) 
CONT AND C(49) C(500) C(510) C(520) 
REM 
DIST 1.54,0.02=C(68) TO C(64) 
CONT C(64) TO C(65), C(64) TO C(66), C(64) TO C(67) 
CONT C(64) TO C(650), C(64) TO C(660), C(64) TO C(670) 
SAME C(64) C(65) C(66) C(67) 
CONT AND C(64) C(650) C(660) C(670) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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