Polyoxometalate-supported transition metal complexes for the oxidative cross-coupling of amines and alcohols.
Pardiwala, Ankita; Desai, Meghal A.; Jangir, Ritambhara; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17207–17220; doi:10.1039/d4dt02289k

data_7717065
_publ_section_title
;
 Polyoxometalate-supported transition metal complexes for the oxidative
 cross-coupling of amines and alcohols.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17207
_journal_page_last               17220
_journal_paper_doi               10.1039/d4dt02289k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Mo6 O19, C12 H36 Co O6 S6'
_chemical_formula_sum            'C12 H36 Co Mo6 O25 S6'
_chemical_formula_weight         1407.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-05
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2024-06-10 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                94.763(4)
_cell_angle_beta                 93.152(4)
_cell_angle_gamma                91.312(4)
_cell_formula_units_Z            1
_cell_length_a                   8.6329(9)
_cell_length_b                   9.2575(9)
_cell_length_c                   12.2531(13)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.8070
_cell_measurement_theta_min      2.0280
_cell_volume                     974.03(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.0
_diffrn_measured_fraction_theta_full 0.998
_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  0.0515
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35080
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.533
_diffrn_reflns_theta_min         2.208
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.687
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1443 before and 0.0752 after correction.
The Ratio of minimum to maximum transmission is 0.6994.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.399
_exptl_crystal_description       block
_exptl_crystal_F_000             683
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.211
_refine_diff_density_max         2.369
_refine_diff_density_min         -2.088
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0726P)^2^+2.1442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4188
_reflns_number_total             4469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02289k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7717064--7717066.cif.'
_cod_database_code               7717065
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.601
_shelx_estimated_absorpt_t_min   0.530
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C4(H4A,
 H4B,H4C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              26655
_shelx_hkl_checksum              81208
_olex2_submission_special_instructions 'No special instructions were received'