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_7717064
_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         'C12 H28 Cu Mo8 N4 O30, 2(C3 H8 N O)'
_chemical_formula_sum            'C18 H44 Cu Mo8 N6 O32'
_chemical_formula_weight         1687.65
_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     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2k8fdp
_audit_creation_date             2024-08-30
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2024-09-03 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                112.753(2)
_cell_angle_beta                 104.637(2)
_cell_angle_gamma                107.424(2)
_cell_formula_units_Z            1
_cell_length_a                   11.6217(2)
_cell_length_b                   11.7346(2)
_cell_length_c                   11.9051(2)
_cell_measurement_reflns_used    16437
_cell_measurement_temperature    296.68(10)
_cell_measurement_theta_max      26.8070
_cell_measurement_theta_min      2.0280
_cell_volume                     1297.20(6)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.68(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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     -5.00  41.00   0.50    2.00    --   16.22 -30.00 -30.00   92
  2  \w      9.00  74.00   0.50    2.00    --   16.22 -15.00  30.00  130
  3  \w     10.00  60.00   0.50    2.00    --   16.22-125.00 -30.00  100
  4  \w    -28.00   6.00   0.50    2.00    --   16.22 -15.00  30.00   68
  5  \w    -37.00  20.00   0.50    2.00    --  -14.97 -94.00  60.00  114
  6  \w    -49.00 -23.00   0.50    2.00    --   16.22 -30.00   0.00   52
  7  \w    -51.00  42.00   0.50    2.00    --   16.22 -61.00   0.00  186
  8  \w    -37.00  22.00   0.50    2.00    --  -14.97 -94.00 -60.00  118
  9  \w    -37.00  22.00   0.50    2.00    --  -14.97 -94.00-120.00  118
 10  \w     11.00  71.00   0.50    2.00    --   16.22-125.00-150.00  120
 11  \w    -41.00  59.00   0.50    2.00    --  -14.97  30.00 -90.00  200
 12  \w    -10.00  85.00   0.50    2.00    --   16.22  61.00-120.00  190
 13  \w    -39.00  55.00   0.50    2.00    --  -14.97  45.00 -60.00  188
 14  \w    -60.00  49.00   0.50    2.00    --   16.22 -83.00 -18.00  218
 15  \w    -55.00 -26.00   0.50    2.00    --   16.22 -30.00 -30.00   58
 16  \w    -91.00  18.00   0.50    2.00    --  -14.97 -83.00 -18.00  218
 17  \w    -59.00 -33.00   0.50    2.00    --   16.22 -15.00  30.00   52
 18  \w    -89.00  10.00   0.50    2.00    --  -14.97 -30.00  60.00  198
 19  \w    -48.00  61.00   0.50    2.00    --  -14.97  83.00 103.00  218
 20  \w    -69.00 -10.00   0.50    2.00    --  -14.97 125.00 -90.00  118
 21  \w    -69.00 -10.00   0.50    2.00    --  -14.97 125.00-150.00  118
 22  \w     14.00  61.00   0.50    2.00    --   16.22  83.00 103.00   94
 23  \w    -69.00 -56.50   0.50    2.00    --  -14.97 125.00 120.00   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      0.0461773000
_diffrn_orient_matrix_UB_12      0.0679558000
_diffrn_orient_matrix_UB_13      0.0221210000
_diffrn_orient_matrix_UB_21      0.0413191000
_diffrn_orient_matrix_UB_22      -0.0262310000
_diffrn_orient_matrix_UB_23      -0.0249014000
_diffrn_orient_matrix_UB_31      -0.0335052000
_diffrn_orient_matrix_UB_32      -0.0071927000
_diffrn_orient_matrix_UB_33      -0.0628694000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22841
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.425
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19670
_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 greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_description       block
_exptl_crystal_F_000             815
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.133
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       0.078(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4645
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0759P)^2^+5.8465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4268
_reflns_number_total             4645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02289k2.cif
_cod_data_source_block           exter213
_cod_depositor_comments
'Adding full bibliography for 7717064--7717066.cif.'
_cod_original_cell_volume        1297.20(5)
_cod_database_code               7717064
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C28 H20 Cu Mo8 O26 N8'
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.613
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C9(H9)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C2(H2A,
 H2B,H2C), C8(H8A,H8B,H8C)
3.c Idealised tetrahedral OH refined as rotating group:
 O17(H17)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84838
_shelx_hkl_checksum              23184
_shelx_fab_checksum              63073
_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 2.850
_oxdiff_exptl_absorpt_empirical_full_min 0.516