Synthesis of cationic molybdenum-cobalt heterometallic clusters protected against hydrolysis by macrocyclic triazacyclononane complexes.
Sugiarto, ?; Tagami, Tomoko; Kawamoto, Keisuke; Hayashi, Yoshihito; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9657–9664; doi:10.1039/c8dt01226a

data_7046860
_publ_section_title
;
 Synthesis of cationic molybdenum-cobalt heterometallic clusters protected
 against hydrolysis by macrocyclic triazacyclononane complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9657
_journal_page_last               9664
_journal_paper_doi               10.1039/c8dt01226a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C12 H30 Co2 Mo3 N6 O12, (C F3 Na O3 S)2, (H2 O)7'
_chemical_formula_sum            'C14 H44 Co2 F6 Mo3 N6 Na2 O25 S2'
_chemical_formula_weight         1326.33
_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_method           SHELXL-2014/7
_audit_update_record
;
2018-06-13 deposited with the CCDC.
2018-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                71.24(1)
_cell_angle_beta                 89.20(1)
_cell_angle_gamma                70.73(1)
_cell_formula_units_Z            2
_cell_length_a                   10.0153(4)
_cell_length_b                   14.7620(6)
_cell_length_c                   15.0806(6)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      72.55
_cell_measurement_theta_min      3.74
_cell_volume                     1982.2(2)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT (Bruker AXS)'
_computing_molecular_graphics    'ShelXle (H?bschle et al., 2011)'
_computing_publication_material  'APEX3 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15369
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.654
_diffrn_reflns_theta_min         3.111
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    16.318
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.2815
_exptl_absorpt_correction_type   'Multi-scan (SADABS; Bruker, 2015)'
_exptl_absorpt_process_details
;
The wR2 (int) value was improved from 
0.1418 to 0.0582 after the absorption corrections by using SADABS program.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.222
_exptl_crystal_description       Block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.281
_refine_diff_density_min         -1.874
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         7484
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+39.7341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7215
_reflns_number_total             7484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01226a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7046860--7046863.cif.'
_cod_original_cell_volume        1982.27(14)
_cod_database_code               7046860
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              3445