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_4511805
_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 H4 Ba3 O24.13 V2'
_chemical_formula_sum            'C10 H4 Ba3 O24.13 V2'
_chemical_formula_weight         1024.19
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4796)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.807(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2382(10)
_cell_length_b                   14.5463(14)
_cell_length_c                   15.2328(14)
_cell_measurement_reflns_used    6094
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.009
_cell_measurement_theta_min      2.675
_cell_volume                     2268.4(4)
_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 0.999
_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  0.0461
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19487
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         1.936
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    6.040
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.765688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0612 before and 0.0374 after correction.
The Ratio of minimum to maximum transmission is 0.7657.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'purplish blue'
_exptl_crystal_colour_primary    'purplish blue'
_exptl_crystal_density_diffrn    2.999
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.459
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         3997
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0322P)^2^+6.0494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                3509
_reflns_number_total             3997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg500888u_si_002.cif
_cod_data_source_block           da67tgas
_cod_depositor_comments
'Adding full bibliography for 4511803--4511805.cif.'
_cod_database_code               4511805
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.531
_olex2_refinement_description
;
1. Restrained distances
 O24-H24B \\sim O24-H24A \\sim O23-H23B \\sim O23-H23A
 with sigma of 0.02
 H24B-H24A \\sim H23A-H23B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uiso(H23A) = Uiso(H23B) = Uiso(H24A) = Uiso(H24B)
3. Others
 Fixed Uiso: O1S(0.025)
;
_shelx_res_checksum              72833
_shelx_hkl_checksum              5721
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'