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_7048873
_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
'C52 H100 Co6 Mo10 N4 O58 P6, 2(C16 H36 N), 4.4(C2 H3 N)'
_chemical_formula_sum            'C92.8 H185.2 Co6 Mo10 N10.4 O58 P6'
_chemical_formula_weight         3873.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-01
_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                74.8370(10)
_cell_angle_beta                 80.3310(10)
_cell_angle_gamma                83.527(2)
_cell_formula_units_Z            1
_cell_length_a                   13.9147(6)
_cell_length_b                   17.0418(7)
_cell_length_c                   17.3781(7)
_cell_measurement_reflns_used    9109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.30
_cell_volume                     3910.7(3)
_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      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0618
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            159209
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         1.488
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0659 before and 0.0542 after correction. The Ratio of minimum to maximum transmission is 0.9121. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       block
_exptl_crystal_F_000             1951
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.789
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         23891
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0556P)^2^+11.3341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16723
_reflns_number_total             23891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00075e2.cif
_cod_data_source_block           fs027
_cod_depositor_comments
'Adding full bibliography for 7048870--7048879.cif.'
_cod_original_formula_sum        'C92.80 H185.20 Co6 Mo10 N10.40 O58 P6'
_cod_database_code               7048873
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O20-H20A = O20-H20B
 0.87 with sigma of 0.01
 H20B-H20A
 1.39 with sigma of 0.02
 N1_1-C1_1
 N1_2-C1_2
 N1_3-C1_3
 N1_4-C1_4
 N1_5-C1_5
 1.16 with sigma of 0.01
 C1_1-C2_1
 C1_2-C2_2
 C1_3-C2_3
 C1_4-C2_4
 C1_5-C2_5
 1.43 with sigma of 0.01
 C40B-C39B \\sim C40A-C39A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2_3) \\sim Ueq, Uanis(C1_3) \\sim Ueq, Uanis(N1_3) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1_5) = Uanis(N1_1)
Uanis(C1_5) = Uanis(C1_1)
Uanis(C2_5) = Uanis(C2_1)
Uanis(C39B) = Uanis(C39A)
Uanis(C40A) = Uanis(C40B)
4. Rigid body (RIGU) restrains
 C43, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, C42, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C39A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H38C)=Sof(H38D)=Sof(C39B)=Sof(H39A)=Sof(H39B)=Sof(C40B)=Sof(H40A)=
 Sof(H40B)=Sof(H40C)=1-FVAR(1)
 Sof(H38A)=Sof(H38B)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40D)=
 Sof(H40E)=Sof(H40F)=FVAR(1)
 Sof(H43C)=Sof(H43D)=Sof(C43B)=Sof(H43H)=Sof(H43I)=Sof(H43J)=1-FVAR(2)
 Sof(H43A)=Sof(H43B)=Sof(C43A)=Sof(H43E)=Sof(H43F)=Sof(H43G)=FVAR(2)
 Fixed Sof: N1(0.5) C1(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) N1(0.25)
 C1(0.25) C2(0.25) H2A(0.25) H2B(0.25) H2C(0.25) N1(0.25) C1(0.25) C2(0.25)
 H2A(0.25) H2B(0.25) H2C(0.25) N1(0.2) C1(0.2) C2(0.2) H2A(0.2) H2B(0.2)
 H2C(0.2)
6.a Riding coordinates:
 O19(H19A,H19B), O12(H12A,H12B), O20(H20A,H20B)
6.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C34(H34A,H34B), C29(H29A,H29B), C33(H33A,
 H33B), C35(H35A,H35B), C37(H37A,H37B), C41(H41A,H41B), C38(H38C,H38D),
 C38(H38A,H38B), C42(H42A,H42B), C39B(H39A,H39B), C39A(H39C,H39D), C43(H43A,
 H43B), C43(H43C,H43D)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C17(H17), C20(H20), C18(H18), C21(H21), C8(H8), C11(H11), C10(H10)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C22(H22A,H22B,H22C), C16(H16A,H16B,H16C), C12(H12C,H12D,H12E), C2(H2A,
 H2B,H2C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C40B(H40A,H40B,H40C),
 C40A(H40D,H40E,H40F), C43A(H43E,H43F,H43G), C43B(H43H,H43I,H43J), C2(H2A,H2B,
 H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              93393
_olex2_submission_original_sample_id CH880
_olex2_submission_special_instructions 'No special instructions were received'