A Novel Series of Materials Composed of Arrays of Vanadium Oxide Container Molecules, {V18O42(X)} (X = H2O, Cl-, Br-): Synthesis and Characterization of [M2(H2N(CH2)2NH2)5][{M(H2N(CH2)2NH2)2}2V18O42(X)]. 9H2O (M = Zn, Cd)
M. Ishaque Khan; Elizabeth Yohannes; Robert J. Doedens; Inorganic Chemistry 42 (2003) 3125–3129; doi:10.1021/ic025889u

data_4313549
_publ_section_title
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 A Novel Series of Materials Composed of Arrays of Vanadium Oxide
 Container Molecules, {V18O42(X)} (X = H2O, Cl-, Br-): Synthesis and
 Characterization of [M2(H2N(CH2)2NH2)5][{M(H2N(CH2)2NH2)2}2V18O42(X)].
 9H2O (M = Zn, Cd)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3125
_journal_page_last               3129
_journal_paper_doi               10.1021/ic025889u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C9 H46 N9 O26 V9 Zn2'
_chemical_formula_weight         1285.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   n/a
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.3320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3723(7)
_cell_length_b                   20.9837(11)
_cell_length_c                   15.8379(8)
_cell_measurement_reflns_used    6095
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.4
_cell_volume                     4078.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '20s frames at 0.3 deg omega increments'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43312
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    3.205
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   'semi-empirical from equivalents'
_exptl_absorpt_process_details   'computed via SADABS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.974
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.258
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         10080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.100P)^2^+40.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.1970
_reflns_number_gt                8950
_reflns_number_total             10080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025889usi20021029_094446.cif
_cod_data_source_block           isk35
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
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_cod_database_code               4313549