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_7048872
_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
'C22 H42 Co3 Mo5 N O29 P3, C16 H36 N, 3.75(C2 H3 N)'
_chemical_formula_sum            'C45.5 H87.25 Co3 Mo5 N5.75 O29 P3'
_chemical_formula_weight         1928.36
_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
_audit_creation_date             2017-08-31
_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                107.6320(10)
_cell_angle_beta                 95.0120(10)
_cell_angle_gamma                101.6640(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7500(4)
_cell_length_b                   16.8554(5)
_cell_length_c                   17.1095(5)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.72
_cell_measurement_theta_min      2.27
_cell_volume                     3653.80(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_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  0.0889
_diffrn_reflns_av_unetI/netI     0.1118
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73920
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.089
_diffrn_reflns_theta_min         1.532
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.636
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6813
_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 0.0578 after correction. The Ratio of minimum to maximum transmission is 0.9130. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       rod
_exptl_crystal_F_000             1937
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.636
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         22705
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      15.259
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0363P)^2^+2.6196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14007
_reflns_number_total             22705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00075e2.cif
_cod_data_source_block           fs057
_cod_depositor_comments
'Adding full bibliography for 7048870--7048879.cif.'
_cod_original_cell_volume        3653.79(19)
_cod_original_formula_sum        'C45.50 H87.25 Co3 Mo5 N5.75 O29 P3'
_cod_database_code               7048872
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.814
_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
 N1_1-C1_1
 N1_2-C1_2
 N1_3-C1_3
 N1_4-C1_4
 1.16 with sigma of 0.01
 C2_1-C1_1
 C2_2-C1_2
 C2_3-C1_3
 C2_4-C1_4
 1.43 with sigma of 0.01
3. Others
 Fixed Sof: N1(0.75) C1(0.75) C2(0.75) H2A(0.75) H2B(0.75) H2C(0.75)
4.a Riding coordinates:
 O7(H7A,H7B), O25(H25A,H25B), O24(H24A,H24B)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C23(H23A,H23B), C24(H24C,H24D), C27(H27A,H27B), C33(H33A,H33B),
 C37(H37A,H37B), C28(H28A,H28B), C31(H31A,H31B), C35(H35A,H35B), C32(H32A,H32B),
  C25(H25C,H25D), C29(H29A,H29B), C36(H36A,H36B)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C18(H18), C15(H15), C17(H17), C4(H4), C5(H5)
4.d Idealised Me refined as rotating group:
 C7(H7C,H7D,H7E), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C22(H22A,H22B,H22C), C34(H34A,H34B,H34C), C30(H30A,H30B,H30C), C38(H38A,
 H38B,H38C), C26(H26A,H26B,H26C), C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C2(H2A,H2B,
 H2C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              19319
_olex2_submission_original_sample_id CH889
_olex2_submission_special_instructions 'No special instructions were received'