Self-assembly of mixed-valence and heterometallic metallocycles: efficient catalysts for the oxidation of alcohols to aldehydes in ambient air.
Lai, Ya-Liang; Wang, Xue-Zhi; Dai, Rui-Rong; Huang, Yong-Liang; Zhou, Xian-Chao; Zhou, Xiao-Ping; Li, Dan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7304–7308; doi:10.1039/d0dt01340d

data_7704312
_publ_section_title
;
 Self-assembly of mixed-valence and heterometallic metallocycles:
 efficient catalysts for the oxidation of alcohols to aldehydes in ambient
 air.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7304
_journal_page_last               7308
_journal_paper_doi               10.1039/d0dt01340d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C33 H36 Cl2 Cu6 N18 O8, Cl O4'
_chemical_formula_sum            'C33 H36 Cl3 Cu6 N18 O12'
_chemical_formula_weight         1364.39
_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             2019-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-05 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                108.253(2)
_cell_angle_beta                 97.505(2)
_cell_angle_gamma                106.236(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4929(2)
_cell_length_b                   14.9760(5)
_cell_length_c                   17.9421(4)
_cell_measurement_reflns_used    12701
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      77.5590
_cell_measurement_theta_min      3.2720
_cell_volume                     2258.23(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.959
_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    -52.00 -26.00   0.50    1.20    --   -2.20 -75.00-162.00   52
  2  \w    -33.00  55.00   0.50    1.20    --   -2.20  75.00 -35.00  176
  3  \w     -4.00  22.00   0.50    1.20    --   -2.20 -75.00-162.00   52
  4  \w     80.00 152.00   0.50   10.00    --  106.30  75.00 -35.00  144
  5  \w     26.00 131.00   0.50   10.00    --  106.30 -75.00-162.00  210
  6  \w    -27.00  37.00   0.50    1.20    --    2.20  82.00-180.00  128
  7  \w      0.00  25.00   0.50    1.20    --    2.20  82.00   0.00   50
  8  \w    -32.00  33.00   0.50    1.20    --    2.20  82.00 150.00  130
  9  \w    -20.00   5.00   0.50    1.20    --    2.20 -75.00-162.00   50
 10  \w    -26.00   0.00   0.50    1.20    --    2.20  82.00 -90.00   52
 11  \w    -30.00  -4.00   0.50    1.20    --    2.20  82.00   0.00   52
 12  \w    -31.00  36.00   0.50    1.20    --    2.20  82.00  60.00  134
 13  \w     18.00  87.00   0.50   10.00    --  106.30 -82.00 150.00  138
 14  \w     21.00 118.00   0.50   10.00    --  106.30 -82.00 -30.00  194
 15  \w     34.00 130.00   0.50   10.00    --  106.30 -38.00-180.00  192
 16  \w     18.00  69.00   0.50   10.00    --  106.30 -82.00 -90.00  102
 17  \w     82.00 141.00   0.50   10.00    --  106.30 -82.00 -90.00  118
 18  \w     84.00 196.00   0.50   10.00    --  106.30  38.00  30.00  224
 19  \w     99.00 125.00   0.50   10.00    --  106.30  82.00-180.00   52
 20  \w    149.00 174.00   0.50   10.00    --  106.30  38.00-150.00   50
 21  \w     98.00 137.00   0.50   10.00    --  106.30 -82.00-150.00   78
 22  \w    100.00 125.00   0.50   10.00    --  106.30 -57.00  90.00   50
 23  \w     26.00  75.00   0.50   10.00    --  106.30 -57.00  90.00   98
 24  \w    137.00 194.00   0.50   10.00    --  106.30  82.00-180.00  114
 25  \w     88.00 113.00   0.50   10.00    --  106.30 -82.00 150.00   50
 26  \w     49.00  74.00   0.50   10.00    --  106.30 -82.00   0.00   50
 27  \w    107.00 133.00   0.50   10.00    --  106.30 -82.00   0.00   52
 28  \w     17.00 139.00   0.50   10.00    --  106.30 -19.00  60.00  244
 29  \w     32.00 109.00   0.50   10.00    --  106.30 -82.00  90.00  154
 30  \w     20.00 128.00   0.50   10.00    --  106.30 -38.00   0.00  216
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0187417000
_diffrn_orient_matrix_UB_12      0.1094210000
_diffrn_orient_matrix_UB_13      0.0116501000
_diffrn_orient_matrix_UB_21      -0.0624186000
_diffrn_orient_matrix_UB_22      0.0116483000
_diffrn_orient_matrix_UB_23      0.0762519000
_diffrn_orient_matrix_UB_31      0.1614246000
_diffrn_orient_matrix_UB_32      0.0340889000
_diffrn_orient_matrix_UB_33      0.0521605000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27245
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.614
_diffrn_reflns_theta_min         3.305
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_description       needle
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0804P)^2^+3.8905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7405
_reflns_number_total             9307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01340d2.cif
_cod_data_source_block           180724a
_cod_depositor_comments
'Adding full bibliography for 7704312--7704315.cif.'
_cod_original_cell_volume        2258.22(11)
_cod_database_code               7704312
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNHClCuO
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.899
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: H01R(0.8) H01S(0.8) H01T(0.2) H01U(0.2) H01(0.8) HB(0.8) HC(0.2)
 HD(0.2) C1(0.8) H1A(0.8) H1B(0.8) C0AA(0.2) H0AB(0.2) H0AC(0.2)
3.a Secondary CH2 refined with riding coordinates:
 C01J(H01F,H01J), C01K(H01K,H01L), C01M(H01M,H01N), C01R(H01R,H01S), C01R(H01T,
 H01U), C01V(H01Y,H), C01W(H01Z,HA), C01X(H01,HB), C01X(HC,HD), C01Z(H0AA,HE),
 C1(H1A,H1B), C0AA(H0AB,H0AC)
3.b Aromatic/amide H refined with riding coordinates:
 C014(H014), C015(H015), C017(H017), C019(H019), C01A(H01A), C01B(H01B),
 C01C(H01C), C01D(H01D), C01E(H01E), C01G(H01G), C01H(H01H), C01I(H01I),
 C01O(H01O), C01P(H01P), C01Q(H01Q), C01S(H01V), C01T(H01W), C01U(H01X)
;
_shelx_res_checksum              75751
_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 1.835
_oxdiff_exptl_absorpt_empirical_full_min 0.748