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_7046861
_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         'C17 H35 Co2 Mo5 O18, (H2 O)4.5'
_chemical_formula_sum            'C17 H44 Co2 Mo5 N7 O22.5'
_chemical_formula_weight         1304.15
_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   geom
_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                90
_cell_angle_beta                 106.07(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2313(6)
_cell_length_b                   22.1991(7)
_cell_length_c                   19.1579(6)
_cell_measurement_reflns_used    9055
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      72.62
_cell_measurement_theta_min      3.33
_cell_volume                     7041.9(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54976
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.651
_diffrn_reflns_theta_min         3.056
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    22.199
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3904
_exptl_absorpt_correction_type   'Multi-scan (SADABS; Bruker, 2015)'
_exptl_absorpt_process_details
;
The wR2 (int) value was improved from 0.1257 to 0.0710 after
the absorption corrections by unisg SADABS program.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.460
_exptl_crystal_description       Block
_exptl_crystal_F_000             5112
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.860
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         13920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+27.5884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12520
_reflns_number_total             13920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01226a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7046860--7046863.cif.'
_cod_original_cell_volume        7041.9(4)
_cod_original_formula_sum        'C17 H44 Co2 Mo5 N7 O22.50'
_cod_database_code               7046861
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              22010