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_4346093
_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 H20 Na2 O21 V2, 2(H2 O)'
_chemical_formula_sum            'C8 H24 Na2 O23 V2'
_chemical_formula_weight         636.13
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5931(5)
_cell_length_b                   10.4332(6)
_cell_length_c                   24.2289(13)
_cell_measurement_reflns_used    8898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.945
_cell_measurement_theta_min      2.514
_cell_volume                     2172.2(2)
_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    'ShelXT (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  0.0647
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            43999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.750
_diffrn_reflns_theta_max         27.949
_diffrn_reflns_theta_min         1.681
_diffrn_source_current           35.0
_diffrn_source_power             1.6
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_description       needle
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 2073 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5225
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0245P)^2^+3.6736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5024
_reflns_number_total             5225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00275_si_002.cif
_cod_data_source_block           navtartm
_cod_database_code               4346093
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O20-H20A = O20-H20B = O21-H21A = O21-H21B = O19-H19B = O19-H19A = O17-H17A =
 O17-H17B = O22-H22B = O22-H22A = O3-H3A = O4-H4A = O14-H14A = O14-H14B = O16-
 H16B = O16-H16A = O23A-H23A = O23A-H23B
 0.84 with sigma of 0.02
 H21A-H21B = H23A-H23B
 1.35 with sigma of 0.01
3. Others
 Sof(O23B)=1-FVAR(1)
 Sof(O23A)=FVAR(1)
4.a Riding coordinates:
 O18(H18A,H18B), O21(H21A,H21B)
4.b Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7)
;
_shelx_res_checksum              83453
_shelx_hkl_checksum              20507
_olex2_submission_special_instructions 'No special instructions were received'