Synthesis of a Spin-Coupled, Mixed-Metal Double Square Grid Complex [(poap-H)4Cu(II)3Fe(III)(NO3)]2(ClO4)4(NO3)4.12H2O (poap = N3-(2-pyridoyl)-2-pyridinecarboxamidrazone) with an S = 3 Ground State, from a Mononuclear Fe(III) Precursor Complex
Zhiqiang Xu; Laurence K. Thompson; Craig J. Matthews; David O. Miller; Andrés E. Goeta; Judith A. K. Howard; Inorganic Chemistry 40 (2001) 2446–2449; doi:10.1021/ic000923v

data_4319593
_publ_section_title
;
 Synthesis of a Spin-Coupled, Mixed-Metal Double Square Grid Complex
 [(poap-H)4Cu(II)3Fe(III)(NO3)]2(ClO4)4(NO3)4.12H2O (poap =
 N3-(2-pyridoyl)-2-pyridinecarboxamidrazone) with an S = 3 Ground State,
 from a Mononuclear Fe(III) Precursor Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2446
_journal_page_last               2449
_journal_paper_doi               10.1021/ic000923v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C96 H100 Cl4 Cu6 Fe2 N46 O52'
_chemical_formula_weight         3364.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 116.3010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5592(7)
_cell_length_b                   32.753(2)
_cell_length_c                   14.9417(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    193.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     6387.5(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      193.2
_diffrn_measurement_device       'Bruker P4CCD'
_diffrn_measurement_method       \w-2\q
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_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -39
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_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33963
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            NONE
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_meas      ?
_exptl_crystal_description       NONE
_exptl_crystal_F_000             3416.00
_exptl_crystal_size_max          0.00
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_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     928
_refine_ls_number_reflns         7017
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0620
_refine_ls_wR_factor_ref         0.0510
_reflns_number_gt                7017
_reflns_number_total             12383
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic000923v_2.cif
_cod_data_source_block           '_Template_texray.inf'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6387.5(5)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C48 H50 Cl2 Cu3 Fe N23 O26 '
_cod_database_code               4319593