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_7048874
_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
'C50 H90 Co6 Mo10 N2 O58 P6, 2(C16 H35.6 N), 3.5(C2 H3 N)'
_chemical_formula_sum            'C89 H171.69 Co6 Mo10 N7.5 O58 P6'
_chemical_formula_weight         3773.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-12
_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                 97.587(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6966(7)
_cell_length_b                   19.5580(9)
_cell_length_c                   23.4785(10)
_cell_measurement_reflns_used    9570
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.46
_cell_volume                     7144.7(6)
_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 0.998
_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  0.0738
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            246867
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.669
_diffrn_reflns_theta_min         1.475
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.671
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0608 before and 0.0535 after correction. The Ratio of minimum to maximum transmission is 0.9153. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_description       block
_exptl_crystal_F_000             3788
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.068
_refine_diff_density_max         2.031
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         20165
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0190P)^2^+42.2267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14960
_reflns_number_total             20165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00075e2.cif
_cod_data_source_block           fs045
_cod_depositor_comments
'Adding full bibliography for 7048870--7048879.cif.'
_cod_original_formula_sum        'C89 H171.69 Co6 Mo10 N7.50 O58 P6'
_cod_database_code               7048874
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.758
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H44A,H44B,H44} of C44, All C(H,H) groups, All C(H,H,H,H)
  groups
 At 1.5 times of:
  All O(H,H) groups, {H44C,H44D,H44E} of C44A, {H41A,H41B,H41C} of C41A,
  {H44F,H44G,H44H} of C44B, {H41D,H41E,H41F} of C41B, {H2A,H2B,H2C} of C2,
  {H1BA,H1BB,H1BC} of C1B, {H2A,H2B,H2C} of C2, {H20C,H20D,H20E} of C20, {H25A,
  H25B,H25C} of C25, {H10A,H10B,H10C} of C10, {H21A,H21B,H21C} of C21, {H11A,
  H11B,H11C} of C11, {H12C,H12D,H12E} of C12, {H33A,H33B,H33C} of C33, {H37A,
  H37B,H37C} of C37, {H23A,H23B,H23C} of C23, {H19C,H19D,H19E} of C19, {H24A,
  H24B,H24C} of C24
2. Restrained distances
 N1_1-C1_1
 N1_2-C1_2
 1.16 with sigma of 0.02
 C1_1-C2_1
 C1_2-C2_2
 1.43 with sigma of 0.02
 H44G_$1-H41C
 2.2 with sigma of 0.02
 H41C-H44G_$1
 2.2 with sigma of 0.02
 C44B-C44 \\sim C44A-C44
 with sigma of 0.02
 C41B-C40 \\sim C41A-C40
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 N2_2, C1A_2, C1B_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1_2, C1_2, C2_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41B, C40, C41A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H44)=Sof(C44B)=Sof(H44F)=Sof(H44G)=Sof(H44H)=1-FVAR(1)
 Sof(H44A)=Sof(H44B)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(H44E)=FVAR(1)
 Sof(N2)=Sof(C1A)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(2)
 Sof(N1)=Sof(C1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(2)
 Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(3)
 Sof(H40A)=Sof(H40B)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(3)
 Fixed Sof: N1(0.75) C1(0.75) C2(0.75) H2A(0.75) H2B(0.75) H2C(0.75)
5.a Riding coordinates:
 O19(H19A,H19B), O20(H20A,H20B), O12(H12A,H12B), C2(H2A,H2B,H2C), C1B(H1BA,
 H1BB,H1BC)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C30(H30A,H30B), C34(H34A,H34B), C36(H36A,H36B), C32(H32A,H32B),
 C35(H35A,H35B), C31(H31A,H31B), C38(H38A,H38B), C39(H39A,H39B), C43(H43A,H43B),
  C42(H42A,H42B), C40(H40A,H40B), C40(H40C,H40D), C44(H44A,H44B)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C17(H17), C14(H14), C15(H15), C4(H4), C16(H16), C5(H5), C8(H8),
 C7(H7), C6(H6), C44(H44)
5.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C19(H19C,H19D,H19E), C20(H20C,H20D,
 H20E), C25(H25A,H25B,H25C), C10(H10A,H10B,H10C), C21(H21A,H21B,H21C), C11(H11A,
 H11B,H11C), C12(H12C,H12D,H12E), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C),
 C41A(H41A,H41B,H41C), C44A(H44C,H44D,H44E), C44B(H44F,H44G,H44H), C41B(H41D,
 H41E,H41F), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              40696
_olex2_submission_original_sample_id PhenAc
_olex2_submission_special_instructions 'No special instructions were received'