Stepwise syntheses and supramolecular assemblies of a series of polyoxovanadate hybrids with various architectures
Huang, Bo; Wang, Nan; Yang, Kang; Ke, Degang; Fang, Yajun; Hu, Xunliang; Wu, Baolin; Xiao, Zicheng; Wu, Pingfan; Wei, Yongge; New Journal of Chemistry 42 (2018) 5853–; doi:10.1039/C7NJ04727D

data_7057101
_publ_section_title
;
 Stepwise syntheses and supramolecular assemblies of a series of
 polyoxovanadate hybrids with various architectures
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5853
_journal_paper_doi               10.1039/C7NJ04727D
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C32 H36 N2 O25 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C64 H108 N4 O25 V6'
_chemical_formula_weight         1639.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-02 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.950(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5838(19)
_cell_length_b                   17.309(2)
_cell_length_c                   16.326(2)
_cell_measurement_reflns_used    2257
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      18.907
_cell_measurement_theta_min      2.353
_cell_volume                     3755.4(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28892
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.273
_diffrn_reflns_theta_min         1.735
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0695 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.9277.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7549
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0944P)^2^+2.9775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.2132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3733
_reflns_number_total             7549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04727d2.cif
_cod_data_source_block           lbxba
_cod_depositor_comments
'Adding full bibliography for 7057098--7057101.cif.'
_cod_original_cell_volume        3755.4(9)
_cod_database_code               7057101
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1AA-C2AA
 1.33 with sigma of 0.01
3. Rigid bond restraints
 C54, C53, C52, C51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1AA \\sim C2AA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), C5(H5A,H5B), C14(H14A,H14B), C51(H51A,H51B),
 C41(H41A,H41B), C31(H31A,H31B), C21(H21A,H21B), C22(H22A,H22B), C52(H52A,H52B),
  C42(H42A,H42B), C23(H23A,H23B), C43(H43A,H43B), C32(H32A,H32B), C33(H33A,
 H33B), C53(H53A,H53B)
5.b Aromatic/amide H refined with riding coordinates:
 N13(H13), C11(H11), C8(H8), C9(H9), C10(H10), C1AA(H1AA)
5.c X=CH2 refined with riding coordinates:
 C2AA(H2AA,H2AB)
5.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C44(H44A,H44B,H44C), C24(H24A,H24B,H24C), C54(H54A,H54B,
 H54C)
;
_olex2_submission_special_instructions 'No special instructions were received'