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_7717066
_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 Ni O6 S6'
_chemical_formula_sum            'C12 H36 Mo6 Ni O25 S6'
_chemical_formula_weight         1407.12
_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             2023-07-28
_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                94.803(2)
_cell_angle_beta                 93.302(2)
_cell_angle_gamma                91.519(2)
_cell_formula_units_Z            1
_cell_length_a                   8.64980(10)
_cell_length_b                   9.2159(3)
_cell_length_c                   12.2140(4)
_cell_measurement_reflns_used    15395
_cell_measurement_temperature    299.1
_cell_measurement_theta_max      26.9190
_cell_measurement_theta_min      2.2090
_cell_volume                     968.14(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_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_environment      air
_diffrn_ambient_temperature      299.1
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -8.00  86.00   0.50    4.00    --   16.22  45.00   0.00  188
  2  \w     -8.00  86.00   0.50    4.00    --   16.22  45.00-120.00  188
  3  \w    -37.00  22.00   0.50    4.00    --  -14.97 -94.00   0.00  118
  4  \w     20.00  82.00   0.50    4.00    --   16.22-144.00 -41.00  124
  5  \w    -37.00  53.00   0.50    4.00    --   16.22 -94.00 -90.00  180
  6  \w    -41.00  59.00   0.50    4.00    --  -14.97  30.00   0.00  200
  7  \w    -40.00 -11.00   0.50    4.00    --   16.22 128.00 114.63   58
  8  \w    -11.00  86.00   0.50    4.00    --   16.22  61.00 120.00  194
  9  \w    -37.00  22.00   0.50    4.00    --  -14.97 -94.00 150.00  118
 10  \w     10.00  71.00   0.50    4.00    --   16.22-126.00 126.00  122
 11  \w    -53.00  42.00   0.50    4.00    --   16.22 -61.00  30.00  190
 12  \w    -69.00  99.00   0.50    4.00    --   16.22   0.00  60.00  336
 13  \w    -69.00 -10.00   0.50    4.00    --  -14.97 125.00 -60.00  118
 14  \w    -81.00 -20.00   0.50    4.00    --  -14.97 144.00  12.00  122
 15  \w    -69.00 -10.00   0.50    4.00    --  -14.97 125.00 120.00  118
 16  \w    -89.00  10.00   0.50    4.00    --  -14.97 -30.00   0.00  198
 17  \w    -85.00  10.00   0.50    4.00    --  -14.97 -45.00 -30.00  190
 18  \w    -37.00  22.00   0.50    4.00    --  -14.97 -94.00-120.00  118
 19  \w    -89.00  10.00   0.50    4.00    --  -14.97 -30.00-150.00  198
 20  \w    -70.00 -57.50   0.50    4.00    --  -14.97 126.00-156.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0169876000
_diffrn_orient_matrix_UB_12      0.0091264000
_diffrn_orient_matrix_UB_13      0.0562386000
_diffrn_orient_matrix_UB_21      -0.0798171000
_diffrn_orient_matrix_UB_22      -0.0136208000
_diffrn_orient_matrix_UB_23      -0.0150436000
_diffrn_orient_matrix_UB_31      0.0096961000
_diffrn_orient_matrix_UB_32      -0.0755149000
_diffrn_orient_matrix_UB_33      0.0044069000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20208
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.977
_diffrn_reflns_theta_min         2.219
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    2.413
_exptl_crystal_description       plate
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.171
_refine_diff_density_max         1.224
_refine_diff_density_min         -1.636
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+2.2549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3612
_reflns_number_total             4044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02289k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7717064--7717066.cif.'
_cod_database_code               7717066
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Mo Ni'
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.544
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C1(H1A,
 H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              21264
_shelx_hkl_checksum              79315
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.309
_oxdiff_exptl_absorpt_empirical_full_min 0.786