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_4348646
_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_absolute_configuration ad
_chemical_formula_moiety
'C16 H16 Co6 N8 O80 P2 W20, C16 H16 Co3 N8 O8, Na O6, 15(O2)'
_chemical_formula_sum            'C32 H32 Co9 N16 Na O124 P2 W20'
_chemical_formula_weight         6917.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-14
_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                 92.743(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1218(5)
_cell_length_b                   44.069(2)
_cell_length_c                   13.7866(7)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.417
_cell_measurement_theta_min      2.679
_cell_volume                     7356.3(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46400
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.68
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    16.687
_exptl_absorpt_correction_T_max  0.3487
_exptl_absorpt_correction_T_min  0.2862
_exptl_crystal_density_diffrn    3.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             6184
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.797
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.249
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.044(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1781
_refine_ls_number_reflns         26848
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                23108
_reflns_number_total             26848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01468_si_002.cif
_cod_data_source_block           p1
_cod_database_code               4348646
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O45W-O44W
 2.75 with sigma of 0.01
 O49W-O44W
 2.75 with sigma of 0.01
 O42W-O49W
 2.75 with sigma of 0.01
 O43W-O49W
 2.75 with sigma of 0.01
 O49W-O45W
 2.75 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Na1 \\sim O42W \\sim O45W \\sim O46W: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.08
O1W \\sim O1WA: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
O2W \\sim O2WA: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
O3W \\sim O3WA: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
Uanis(O19) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C14)
\\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: O4W(0.5) O4WA(0.5) O3W(0.3) O3WA(0.7) O2W(0.5) O2WA(0.5) O5W(0.5)
 O5WA(0.5) O1W(0.5) O1WA(0.5) O6W(0.5) O6WA(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
;
_olex2_submission_special_instructions 'No special instructions were received'