Assembly, disassembly and reassembly: a "top-down" synthetic strategy towards hybrid, mixed-metal {Mo<sub>10</sub>Co<sub>6</sub>} POM clusters.
Healy, Colm; Steuber, Friedrich W.; Wix, Paul; Macreadie, Lauren K.; Kathalikkattil, Amal Cherian; Schmitt, Wolfgang; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3018–3027; doi:10.1039/c9dt00075e

data_7048870
_publ_section_title
;
 Assembly, disassembly and reassembly: a &quot;top-down&quot; synthetic
 strategy towards hybrid, mixed-metal {Mo<sub>10</sub>Co<sub>6</sub>} POM
 clusters.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3018
_journal_page_last               3027
_journal_paper_doi               10.1039/c9dt00075e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C58 H96 Co6 Mo10 N4 O58 P6, 2(C16 H36 N)'
_chemical_formula_sum            'C90 H168 Co6 Mo10 N6 O58 P6'
_chemical_formula_weight         3761.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-02 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.8360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7038(18)
_cell_length_b                   24.446(2)
_cell_length_c                   28.467(3)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.188
_cell_measurement_theta_min      2.244
_cell_volume                     14208(2)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            55974
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.304
_diffrn_reflns_theta_min         1.521
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0605 before and 0.0443 after correction. The Ratio of minimum to maximum transmission is 0.7921. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       fragment
_exptl_crystal_F_000             7544
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.718
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         17629
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0902P)^2^+146.7333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11589
_reflns_number_total             17629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00075e2.cif
_cod_data_source_block           ch764_a
_cod_depositor_comments
'Adding full bibliography for 7048870--7048879.cif.'
_cod_database_code               7048870
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.752
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H0CA_$1-H0CA_$2
 2 with sigma of 0.02
 H0CA-H0CA_$3
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1AA) = Uanis(C2AA) = Uanis(C7BA) = Uanis(C3AA) = Uanis(C14)
Uanis(N2A) = Uanis(C0AB) = Uanis(C27A) = Uanis(C02H) = Uanis(C02C) = Uanis(C25)
Uanis(N2) = Uanis(C0AA) = Uanis(C27) = Uanis(C02G) = Uanis(C02B) = Uanis(C25A)
Uanis(C7AA) = Uanis(C8AA) = Uanis(C9AA) = Uanis(C0BA) = Uanis(C1BA) =
Uanis(C2BA)
Uanis(C5BA) = Uanis(C40)
Uanis(N1AA) = Uanis(C3) = Uanis(C6BA) = Uanis(C5BA) = Uanis(C40)
Uanis(N1AA) = Uanis(C1AA) = Uanis(C39) = Uanis(C4BA) = Uanis(C8BA)
4. Rigid body (RIGU) restrains
 C4AA, C5AA, C9BA, C0CA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C25A)=Sof(H25A)=Sof(N2A)=Sof(C0AB)=Sof(H0AB)=Sof(C27A)=Sof(H27C)=
 Sof(C02H)=Sof(H02H)=Sof(C02C)=Sof(H02C)=1-FVAR(1)
 Sof(N2)=Sof(C0AA)=Sof(H0AA)=Sof(C27)=Sof(H27)=Sof(C02G)=Sof(H02G)=Sof(C02B)=
 Sof(H02B)=Sof(C25)=Sof(H25)=FVAR(1)
6.a Rotating group:
 O26(H26A,H26B), O27(H27A,H27B), O5(H5A,H5B)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2AA(H2AA,H2AB), C3AA(H3AA,H3AB), C39(H39A,H39B), C1AA(H1AA,
 H1AB), C6BA(H6BA,H6BB), C5BA(H5BA,H), C7BA(H7BA,H7BB), C4BA(H4BA,H4BB),
 C4AA(H4AA,H4AB), C5AA(H5AA,H5AB), C9BA(H9BA,H9BB)
6.c Me refined with riding coordinates:
 C0CA(H0CA,H0CB,H0CC)
6.d Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C27(H27), C02G(H02G), C02B(H02B), C25A(H25A), C22(H22), C21(H21),
 C24(H24), C23(H23), C20(H20), C0AB(H0AB), C27A(H27C), C02H(H02H), C02C(H02C),
 C25(H25), C9AA(H9AA), C0BA(H0BA), C1BA(H1BA), C2BA(H2BA), C8AA(H8AA)
6.e Fitted hexagon refined as free rotating group:
 N2(C0AA,C27,C02G,C02B,C25A), N2A(C0AB,C27A,C02H,C02C,C25), C9AA(C0BA,C1BA,
 C2BA,C7AA,C8AA)
6.f Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C),
 C9(H9A,H9B,H9C), C5(H5C,H5D,H5E), C3BA(H3BA,H3BB,H3BC), C1(H1A,H1B,H1C),
 C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C40(H40A,H40B,H40C), C8BA(H8BA,H8BB,H8BC)
;
_olex2_submission_special_instructions 'No special instructions were received'