Observation of Multiple Crystal-to-Crystal Transitions in a New Reduced Vanadium Oxalate Hybrid Material, Ba3[(VO)2(C2O4)5(H2O)6]·(H2O)3, Prepared via a Mild, Two-Step Hydrothermal Method
Abeysinghe, Dileka; Smith, Mark D.; Yeon, Jeongho; Morrison, Gregory; zur Loye, Hans-Conrad; Crystal Growth & Design 14 (2014) 4749–; doi:10.1021/cg500888u

data_4511804
_publ_section_title
;
 Observation of Multiple Crystal-to-Crystal Transitions in a New Reduced
 Vanadium Oxalate Hybrid Material, Ba3[(VO)2(C2O4)5(H2O)6]&#x00B7;(H2O)3,
 Prepared via a Mild, Two-Step Hydrothermal Method
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4749
_journal_paper_doi               10.1021/cg500888u
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C10 H8 Ba3 O26 V2, 2(H2 O)'
_chemical_formula_sum            'C10 H12 Ba3 O28 V2'
_chemical_formula_weight         1094.10
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.718(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2354(19)
_cell_length_b                   15.455(3)
_cell_length_c                   17.536(3)
_cell_measurement_reflns_used    5995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.391
_cell_measurement_theta_min      2.406
_cell_volume                     2741.9(9)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.631 (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16453
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         2.350
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    5.016
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.694363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0644 before and 0.0241 after correction.
The Ratio of minimum to maximum transmission is 0.6944.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.650
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+7.1923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2803
_reflns_number_total             2824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg500888u_si_002.cif
_cod_data_source_block           da1108as
_cod_depositor_comments
'Adding full bibliography for 4511803--4511805.cif.'
_cod_database_code               4511804
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.315
_shelx_estimated_absorpt_t_min   0.239
_olex2_refinement_description
;
;
_shelx_res_checksum              76145
_shelx_hkl_checksum              85541
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'