{Fe3Nb25} cluster based on an Fe-centred Keggin unit.
Liang, Zhijie; Wang, Ke; Zhang, Dongdi; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1368–1371; doi:10.1039/c6dt04223f

data_7041645
_publ_section_title
;
 {Fe3Nb25} cluster based on an Fe-centred Keggin unit.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1368
_journal_page_last               1371
_journal_paper_doi               10.1039/c6dt04223f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'Fe3 K3 Na2 Nb25 O86.5, 2(C2 H10 N2), 6.5(O)'
_chemical_formula_sum            'C4 H53 Fe3 K3 N4 Na2 Nb25 O93'
_chemical_formula_weight         4299.08
_chemical_name_systematic
;
 ? 
;
_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     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1mq80m
_audit_creation_date             2016-11-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-12-12 deposited with the CCDC.
2017-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                95.865(5)
_cell_angle_beta                 98.824(3)
_cell_angle_gamma                119.937(3)
_cell_formula_units_Z            2
_cell_length_a                   16.251(3)
_cell_length_b                   16.270(5)
_cell_length_c                   26.665(5)
_cell_measurement_reflns_used    5849
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.51
_cell_volume                     5904(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0533
_diffrn_reflns_av_unetI/netI     0.1085
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30414
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.523
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.889
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0847 before and 0.0554 after correction.
The Ratio of minimum to maximum transmission is 0.5230.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4062
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.908
_refine_diff_density_min         -2.844
_refine_diff_density_rms         0.452
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         20737
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1429
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1665P)^2^+104.5408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2547
_refine_ls_wR_factor_ref         0.2952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13450
_reflns_number_total             20737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04223f2.cif
_cod_data_source_block           njy1
_cod_depositor_comments
'Adding full bibliography for 7041469--7041645.cif.'
_cod_original_cell_volume        5905(2)
_cod_database_code               7041645
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Restrained distances
 N1-C1 = C1-C2 = C2-N2 = C3-C4
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N3 \\sim C3: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
C1 \\sim N1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C2 \\sim N2: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O66) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O36) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Nb21(0.33333) Fe2(0.66666) Nb26(0.33333) Fe3(0.66666)
 Nb27(0.33333) Fe4(0.66666) O13W(0.5) O14W(0.5) O15W(0.5) O16W(0.5) O17W(0.5)
 O18W(0.5) O19W(0.5) O20W(0.5) O21W(0.5) O22W(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2D,H2E), C3(H3D,H3E), C4(H4D,H4E)
5.b Me refined with riding coordinates:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'