A new tetra-Zr(iv)-substituted polyoxotungstate aggregate.
Li, Hai-Lou; Wang, Yue-Lin; Zhang, Zhong; Yang, Bai-Feng; Yang, Guo-Yu; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14017–14024; doi:10.1039/c8dt03317j

data_7047482
_publ_section_title
;
 A new tetra-Zr(iv)-substituted polyoxotungstate aggregate.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14017
_journal_page_last               14024
_journal_paper_doi               10.1039/c8dt03317j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C4 H16 N2 Na6 O137 P6 Sb2 W28 Zr4, 9(O), 4(C2 H8 N)'
_chemical_formula_sum            'C12 H160 N6 Na6 O172 P6 Sb2 W28 Zr4'
_chemical_formula_weight         9221.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-05 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                94.068(2)
_cell_angle_beta                 103.151(2)
_cell_angle_gamma                102.989(2)
_cell_formula_units_Z            1
_cell_length_a                   14.1747(4)
_cell_length_b                   17.7610(5)
_cell_length_c                   19.7781(6)
_cell_measurement_reflns_used    5315
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2180
_cell_measurement_theta_min      3.8200
_cell_volume                     4685.4(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0748
_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       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44894
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         2.915
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.779
_exptl_absorpt_correction_T_max  0.1421
_exptl_absorpt_correction_T_min  0.0951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needlelike
_exptl_crystal_F_000             4140
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.573
_refine_diff_density_min         -2.751
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         16601
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12002
_reflns_number_total             16601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03317j2.cif
_cod_data_source_block           q
_cod_depositor_comments
;
Adding full bibliography for 7047482.cif.

2023-11-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C6 H80 N3 Na3 O86 P3 Sb W14 Zr2'
_cod_original_formula_weight         4610.70
_cod_original_formula_moiety
'C2 H8 N Na3 O68.5 P3 Sb W14 Zr2, 4.5(O), 2(C2 H8 N)'
_cod_original_formula_units_Z            2
_cod_database_code               7047482
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.142
_shelx_estimated_absorpt_t_min   0.095
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-N1 = N1-C2 = N3-C5 = N3-C6
 1.48 with sigma of 0.01
 C3-N2 = N2-C4
 1.48 with sigma of 0.01
3. Others
 Fixed Sof: Na3(0.6) Na4(0.4) O1W(0.5) O2W(0.5) O6W(0.5) O8W(0.5) O10W(0.5)
 O11W(0.5) O12W(0.5) O15W(0.5)
 Fixed Uiso: N2(0.08567) C5(0.0862) C6(0.08739) N3(0.08645)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2D,H2E), N3(H3A,H3B)
4.b Me refined with riding coordinates:
 C1(H1C,H1D,H1E), C2(H2A,H2B,H2C), C3(H3C,H3D,H3E), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              28593
_olex2_submission_special_instructions 'No special instructions were received'