pH-Controlled assembly of two novel Dawson-sandwiched clusters involving the in situ reorganization of trivacant α-[P2W15O56](12-) into divacant α-[P2W16O57](8.).
Guo, Ling-Yu; Jagodič, Marko; Zeng, Su-Yuan; Wang, Zhi; Shi, Zhi-Qiang; Wang, Xing-Po; Tung, Chen-Ho; Sun, Di; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8404–8411; doi:10.1039/c6dt00793g

data_7039007
_publ_section_title
;
 pH-Controlled assembly of two novel Dawson-sandwiched clusters involving
 the in situ reorganization of trivacant \a-[P2W15O56](12-) into divacant
 \a-[P2W16O57](8.).
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8404
_journal_page_last               8411
_journal_paper_doi               10.1039/c6dt00793g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'Co3 O114 P4 W31, 6(C10 H16 N4), 12(O)'
_chemical_formula_sum            'C60 H96 Co3 N24 O126 P4 W31'
_chemical_formula_weight         9169.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-05 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.4003(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.592(3)
_cell_length_b                   14.2596(17)
_cell_length_c                   24.846(3)
_cell_measurement_reflns_used    5428
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.279
_cell_measurement_theta_min      2.454
_cell_volume                     8112.1(17)
_computing_cell_refinement       'APEX2 (Bruker,2005)'
_computing_data_collection       'APEX2 (Bruker,2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND  (Brandenburg, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            45258
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.451
_exptl_absorpt_coefficient_mu    22.327
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.8059.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    3.754
_exptl_crystal_description       block
_exptl_crystal_F_000             8134
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6009
_refine_diff_density_max         2.514
_refine_diff_density_min         -2.903
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         15970
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+7.8885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10803
_reflns_number_total             15970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00793g2.cif
_cod_data_source_block           p2
_cod_depositor_comments
'Adding full bibliography for 7039006--7039007.cif.'
_cod_original_cell_volume        8112.0(17)
_cod_database_code               7039007
_shelx_estimated_absorpt_t_max   0.401
_shelx_estimated_absorpt_t_min   0.214
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Co1, W1}
3. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(Co1) = Uanis(W1)
4. Others
 Fixed Sof: W1(0.5) Co1(0.5) O6W(0.5) O6WA(0.5)
5.a Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C6(H6A,H6B,H6C)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N7(H7), N8(H8), N1(H1), N2(H2), N3(H3), N4(H4), N9(H9),
 N10(H10), N11(H11), N12(H12)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C1(H1A,H1B,
 H1C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'