A Pyridazine-Bridged Sandwiched Cluster Incorporating Planar Hexanuclear Cobalt Ring and Bivacant Phosphotungstate.
Guo, Ling-Yu; Zeng, Su-Yuan; Jagličić, Zvonko; Hu, Qi-Dong; Wang, Shi-Xuan; Wang, Zhi; Sun, Di; Inorganic chemistry 55 (2016) 9006–9011; doi:10.1021/acs.inorgchem.6b01468

data_4348647
_publ_section_title
;
 A Pyridazine-Bridged Sandwiched Cluster Incorporating Planar Hexanuclear
 Cobalt Ring and Bivacant Phosphotungstate.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9006
_journal_page_last               9011
_journal_paper_doi               10.1021/acs.inorgchem.6b01468
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'O62 P2 W18, 4(C4 H6 N2), C8 N4, 6(O)'
_chemical_formula_sum            'C24 H35 N12 O66 P2 W18'
_chemical_formula_weight         4918.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.5448(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0063(15)
_cell_length_b                   21.093(2)
_cell_length_c                   14.0094(15)
_cell_measurement_reflns_used    7477
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.442
_cell_measurement_theta_min      2.585
_cell_volume                     3849.7(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25310
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.482
_exptl_absorpt_coefficient_mu    26.926
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1403 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.3527.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    4.243
_exptl_crystal_description       rod
_exptl_crystal_F_000             4306
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.034
_refine_diff_density_min         -3.102
_refine_diff_density_rms         0.441
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         6981
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+49.6750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5677
_reflns_number_total             6981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01468_si_002.cif
_cod_data_source_block           p2
_cod_database_code               4348647
_shelx_estimated_absorpt_t_max   0.174
_shelx_estimated_absorpt_t_min   0.075
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Shared sites
{N7, C7A}
{N8, C8A}
{N5, C5A}
{N6, C6A}
3. Restrained planarity
 C2, N5, N6, C6A, C1, C5A
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
C2 \\sim N5 \\sim N6 \\sim C6A \\sim C1 \\sim C5A \\sim C4 \\sim N7 \\sim C7A
\\sim N8 \\sim C8A \\sim C3: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.08
Uanis(P2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(N7) = Uanis(C7A)
Uanis(N8) = Uanis(C8A)
Uiso(N5) = Uiso(C5A)
Uiso(N6) = Uiso(C6A)
5. Others
 Fixed Sof: N5(0.5) N6(0.5) N7(0.5) N8(0.5) C5A(0.5) C6A(0.5) C7A(0.5) C8A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C5(H5), C6(H6), C7(H7), C8(H8), N1(H1), N2(H2), C9(H9),
 C10(H10), C11(H11), C12(H12)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'