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_7048877
_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
'2(C84 H122 Co6 Mo10 N2 O58 P6), 4(C16 H34 N), 4(C2 H3 N)'
_chemical_formula_sum            'C240 H354 Co12 Mo20 N12 O116 P12'
_chemical_formula_weight         8260.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-26
_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                 91.4630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.7884(13)
_cell_length_b                   28.1953(12)
_cell_length_c                   19.9483(8)
_cell_measurement_reflns_used    9428
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      2.18
_cell_volume                     16749.0(12)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0738
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            157139
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.783
_diffrn_reflns_theta_min         1.368
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0591 before and 0.0535 after correction. The Ratio of minimum to maximum transmission is 0.8991. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       fragment
_exptl_crystal_F_000             8300
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.770
_refine_diff_density_min         -2.139
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         16357
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.292
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+355.1046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.2192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10107
_reflns_number_total             16357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00075e2.cif
_cod_data_source_block           ch763pw_a
_cod_depositor_comments
'Adding full bibliography for 7048870--7048879.cif.'
_cod_database_code               7048877
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.825
_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
 C48-C49
 1.54 with sigma of 0.01
 C49-C50
 1.54 with sigma of 0.01
 C50-C51
 1.54 with sigma of 0.01
 C50-C52
 1.54 with sigma of 0.01
 C52-C53
 1.54 with sigma of 0.01
 C53-C54
 1.54 with sigma of 0.01
 C54-C48
 1.54 with sigma of 0.01
 C21-C26
 1.54 with sigma of 0.01
 C26_$1-C25_$1
 1.54 with sigma of 0.01
 N1-C1
 1.334 with sigma of 0.02
 N1-C5
 1.334 with sigma of 0.02
 C5-C4
 1.377 with sigma of 0.02
 C4-C3
 1.377 with sigma of 0.02
 C3-C2
 1.377 with sigma of 0.02
 C2-C1
 1.377 with sigma of 0.02
 N2-C32
 1.334 with sigma of 0.02
 N2-C28
 1.334 with sigma of 0.02
 C28-C29
 1.377 with sigma of 0.02
 C30-C29
 1.377 with sigma of 0.02
 C30-C31
 1.377 with sigma of 0.02
 C31-C32
 1.377 with sigma of 0.02
 C25_$1-C24_$1
 1.54 with sigma of 0.01
 C24-C23
 1.54 with sigma of 0.01
 C24-C27
 1.54 with sigma of 0.01
 C27-C25_$2
 1.54 with sigma of 0.02
 C27-C26_$2
 2.55 with sigma of 0.01
 C25-C27
 1.54 with sigma of 0.01
 C59-C57
 1.54 with sigma of 0.01
 C48-C53
 2.55 with sigma of 0.01
 C54-C52
 2.55 with sigma of 0.01
 C53-C50
 2.55 with sigma of 0.01
 C52-C49
 2.55 with sigma of 0.01
 C50-C48
 2.55 with sigma of 0.01
 C49-C51
 2.55 with sigma of 0.01
 C51-C52
 2.55 with sigma of 0.01
 C21-C25
 2.55 with sigma of 0.01
 C25-C23
 2.55 with sigma of 0.01
 N1-C4
 2.395 with sigma of 0.04
 N1-C2
 2.395 with sigma of 0.04
 C1-C3
 2.363 with sigma of 0.04
 C5-C3
 2.363 with sigma of 0.04
 C2-C4
 2.363 with sigma of 0.04
 C5-C1
 2.363 with sigma of 0.04
 N2-C31
 2.395 with sigma of 0.04
 N2-C29
 2.395 with sigma of 0.04
 C28-C32
 2.363 with sigma of 0.04
 C32-C30
 2.363 with sigma of 0.04
 C28-C30
 2.363 with sigma of 0.04
 C31-C29
 2.363 with sigma of 0.04
 C24-C27
 2.55 with sigma of 0.01
 C26_$1-C24_$1
 2.55 with sigma of 0.01
 C26-C27
 2.55 with sigma of 0.01
 C27-C24
 2.55 with sigma of 0.01
 C27-C24_$2
 2.55 with sigma of 0.01
3. Restrained planarity
 N1, C1, C2, C3, C4, C5
 with sigma of 0.01
 N2, C32, C31, C30, C29, C28
 with sigma of 0.01
4. Rigid bond restraints
 Co3, O29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Co3 \\sim O29: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O27) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C51) = Uanis(C48) = Uanis(C49) = Uanis(C54) = Uanis(C50) = Uanis(C52) =
Uanis(C53)
Uanis(C29) = Uanis(C30) = Uanis(C28) = Uanis(C31) = Uanis(C32)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5)
Uanis(C22) = Uanis(C26) = Uanis(C21) = Uanis(C25) = Uanis(C24) = Uanis(C23) =
Uanis(C27)
6. Rigid body (RIGU) restrains
 C67, C66, C65, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C68, C69, C70, C71
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: O10(0.5) H10A(0.5) H10B(0.5) N1(0.5) C1(0.5) H1(0.5) C2(0.5)
 H2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) H22A(0.5) H22B(0.5)
 O27(0.5) H27C(0.5) H27D(0.5) N2(0.5) H54A(0.5) H54B(0.5) C29(0.5) H29(0.5)
 C30(0.5) H30(0.5) C28(0.5) H28(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5)
 H57(0.61084) H57A(0.38916) C58(0.61084) H58A(0.61084) H58B(0.61084)
 H58C(0.61084) C59(0.38916) H59A(0.38916) H59B(0.38916) H59C(0.38916)
8.a Rotating group:
 O10(H10A,H10B), O12(H12A,H12B), O27(H27C,H27D), O29(H29A,H29B)
8.b Ternary CH refined with riding coordinates:
 C8(H8), C10(H10), C13(H13), C25(H25), C23(H23), C50(H50), C53(H53), C37(H37),
 C35(H35), C40(H40)
8.c Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C7(H7A,H7B), C11(H11A,H11B), C9(H9A,H9B), C26(H26A,H26B),
 C15(H15A,H15B), C12(H12C,H12D), C14(H14A,H14B), C24(H24A,H24B), C27(H27A,H27B),
  C49(H49A,H49B), C54(H54A,H54B), C51(H51A,H51B), C52(H52A,H52B), C34(H34A,
 H34B), C39(H39A,H39B), C36(H36A,H36B), C38(H38A,H38B), C41(H41A,H41B),
 C42(H42A,H42B), C65(H65A,H65B), C55(H55A,H55B), C60(H60A,H60B), C64(H64A,H64B),
  C68(H68A,H68B), C56(H56A,H56B), C61(H61A,H61B), C62(H62A,H62B), C69(H69A,
 H69B), C70(H70A,H70B)
8.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C18(H18), C20(H20), C19(H19),
 C29(H29), C30(H30), C45(H45), C47(H47), C46(H46), C28(H28), C31(H31), C32(H32),
  C66(H66), C57(H57), C57(H57A)
8.e Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C71(H71A,H71B,H71C), C67(H67A,H67B,H67C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C73(H73A,H73B,H73C)
;
_olex2_submission_special_instructions 'No special instructions were received'