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_4511803
_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 H12 Ba3 O28 V2, 3(H2 O)'
_chemical_formula_sum            'C10 H18 Ba3 O31 V2'
_chemical_formula_weight         1148.14
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.413(2)
_cell_angle_gamma                90
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_cell_length_a                   10.7250(11)
_cell_length_b                   15.2040(16)
_cell_length_c                   17.3541(18)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.320
_cell_measurement_theta_min      2.345
_cell_volume                     2791.7(5)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.631 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
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_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_max       18
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_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16423
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.941
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.732
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
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_refine_diff_density_min         -2.200
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.360
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.360
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+83.3190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                2719
_reflns_number_total             2867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg500888u_si_002.cif
_cod_data_source_block           da1067bs
_cod_depositor_comments
'Adding full bibliography for 4511803--4511805.cif.'
_cod_database_code               4511803
_shelx_estimated_absorpt_t_min   0.589
_shelx_estimated_absorpt_t_max   0.790
_shelxl_version_number           2013-4
_shelx_res_checksum              70963
_shelx_hkl_checksum              8353