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_4348645
_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
'C16 H30 Co2 N8 Na2 O120 P4 W32, 8(C4 H5 N2), 10(O)'
_chemical_formula_sum            'C48 H70 Co2 N24 Na2 O130 P4 W32'
_chemical_formula_weight         9234.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.2102(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.444(2)
_cell_length_b                   23.888(3)
_cell_length_c                   20.171(3)
_cell_measurement_reflns_used    2682
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.635
_cell_measurement_theta_min      2.482
_cell_volume                     8382.6(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14740
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    22.198
_exptl_absorpt_correction_T_max  0.2150
_exptl_absorpt_correction_T_min  0.0952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             8140
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.300
_refine_diff_density_min         -1.938
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         14740
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                8187
_reflns_number_total             14740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01468_si_003.cif
_cod_data_source_block           p3
_cod_original_cell_volume        8383(2)
_cod_database_code               4348645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{Na1, W1A}
{W1, Na1A}
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.02
Uanis(O5W) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(Na1) = Uanis(W1A)
Uanis(W1) = Uanis(Na1A)
4. Others
 Fixed Sof: W1(0.65) W1A(0.35) Na1(0.35) Na1A(0.65)
5.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
5.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C2(H2), C3(H3), C4(H4A), C5(H5), C6(H6), C7(H7), C8(H8),
 N9(H9), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C18(H18), C17(H17),
 N11(H11), C20(H20), N7(H7A), C21(H21), C22(H22), C23(H23), C24(H24), N6(H6A),
 C9(H9A), C10(H10), C11(H11A), C12(H12)
5.c Fitted hexagon refined as free rotating group:
 C19(C18,C17,N11,N12,C20)
;
_olex2_submission_special_instructions 'No special instructions were received'