Effects of Reaction Gel Dehydration on the Synthesis of Cu(NC5H5)4VOF4and [Cu(NC5H5)4VOF4][Cu(NC5H5)4(H2O)VOF4]·H2O
Welk, Margaret E.; Stern, Charlotte L.; Poeppelmeier, Kenneth R.; Norquist, Alexander J.; Crystal Growth & Design 7 (2007) 956–; doi:10.1021/cg0609062

data_4504185
_publ_section_title
;
 Effects of Reaction Gel Dehydration on the Synthesis of Cu(NC5H5)4VOF4and
 [Cu(NC5H5)4VOF4][Cu(NC5H5)4(H2O)VOF4]&#x00B7;H2O
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              956
_journal_paper_doi               10.1021/cg0609062
_journal_volume                  7
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H20 Cu1 F4 N4 O1 V1'
_chemical_formula_sum            'C20 H20 Cu F4 N4 O V'
_chemical_formula_weight         522.88
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-10-05
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.5023(5)
_cell_length_b                   13.0806(7)
_cell_length_c                   31.0970(16)
_cell_measurement_reflns_used    2500
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     4272.0(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            36728
_diffrn_reflns_theta_full        27.452
_diffrn_reflns_theta_max         28.301
_diffrn_reflns_theta_min         2.487
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_meas      1.616(5)
_exptl_crystal_density_method    'floatation pycnometry'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.39
_refine_ls_abs_structure_details 'Flack (1983), 2203 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.389(15)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.001018
_refine_ls_structure_factor_coef Fsqd
_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: 
 4.71 6.82 3.56 1.05 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0779
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0673
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                3379
_reflns_number_total             5096
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.067810(12)
_oxford_structure_analysis_title '10051054 Compound X'
_cod_data_source_file            cg0609062si20061211_025118.cif
_cod_data_source_block           Cu(pyridine)~4~VOF~4~_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2 2 21 '
_cod_original_formula_sum        'C20 H20 Cu1 F4 N4 O1 V1'
_cod_database_code               4504185