Crystal growth of four oxovanadium(IV) tartrates prepared via a mild two-step hydrothermal method: observation of spin-dimer behavior and second harmonic generation.
Cortese, Anthony J.; Wilkins, Branford; Smith, Mark D.; Yeon, Jeongho; Morrison, Gregory; Tran, T. Thao; Halasyamani, P. Shiv; zur Loye, Hans-Conrad; Inorganic chemistry 54 (2015) 4011–4020; doi:10.1021/acs.inorgchem.5b00275

data_4346091
_publ_section_title
;
 Crystal growth of four oxovanadium(IV) tartrates prepared via a mild
 two-step hydrothermal method: observation of spin-dimer behavior and
 second harmonic generation.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4011
_journal_page_last               4020
_journal_paper_doi               10.1021/acs.inorgchem.5b00275
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H12 O17 Rb2 V2, H2 O'
_chemical_formula_sum            'C8 H14 O18 Rb2 V2'
_chemical_formula_weight         671.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-28
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9061(8)
_cell_length_b                   10.2647(11)
_cell_length_c                   22.814(2)
_cell_measurement_reflns_used    7786
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.67
_cell_volume                     1851.4(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26955
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.79
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    6.327
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.791986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0580 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.7920.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4431
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+0.3302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0543
_reflns_number_gt                4174
_reflns_number_total             4431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00275_si_002.cif
_cod_data_source_block           ac1112bs
_cod_original_cell_volume        1851.5(3)
_cod_database_code               4346091
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O17-H17A = O17-H17B = O13-H13A = O13-H13B = O18-H18A = O18-H18B = O15-H15B =
 O15-H15A
 0.84 with sigma of 0.02
 O3-H3 = O4-H4
 0.84 with sigma of 0.02
 H15B-H15A
 1.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(H17A) = Uiso(H17B)
Uiso(H18B) = Uiso(H18A)
4.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3A), C6(H6), C7(H7)
;