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_7704313
_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         'C36 H41.33 Cu6 N18, 3(Cl O4)'
_chemical_formula_sum            'C36 H41.33 Cl3 Cu6 N18 O12'
_chemical_formula_weight         1405.79
_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                112.780(2)
_cell_angle_beta                 93.5500(10)
_cell_angle_gamma                102.5950(10)
_cell_formula_units_Z            2
_cell_length_a                   9.33780(10)
_cell_length_b                   16.3060(3)
_cell_length_c                   17.6821(3)
_cell_measurement_reflns_used    16779
_cell_measurement_temperature    102(3)
_cell_measurement_theta_max      77.2820
_cell_measurement_theta_min      2.7170
_cell_volume                     2390.32(8)
_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      102(3)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_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    -54.00 -27.00   0.50    1.00    --   -0.90 -63.00-158.00   54
  2  \w     -5.00  53.00   0.50    1.00    --   -0.90  63.00 -21.00  116
  3  \w      8.00  33.00   0.50    1.00    --    0.90  63.00 -21.00   50
  4  \w     78.00 132.00   0.50   10.00    --  105.10  63.00 -21.00  108
  5  \w     74.00 118.00   0.50   10.00    --  105.10 -63.00-158.00   88
  6  \w    -32.00  38.00   0.50    1.00    --    0.90  82.00-120.00  140
  7  \w    -39.00  33.00   0.50    1.00    --    0.90 -82.00 150.00  144
  8  \w    -31.00  47.00   0.50    1.00    --    0.90  77.00-180.00  156
  9  \w     -1.00  48.00   0.50    1.00    --    0.90  77.00 120.00   98
 10  \w    -25.00  17.00   0.50    1.00    --    0.90  82.00 -90.00   84
 11  \w     16.00 138.00   0.50   10.00    --  105.10 -19.00 -30.00  244
 12  \w     26.00 138.00   0.50   10.00    --  105.10 -82.00-150.00  224
 13  \w     16.00 128.00   0.50   10.00    --  105.10 -38.00-150.00  224
 14  \w     81.00 107.00   0.50   10.00    --  105.10 -82.00 120.00   52
 15  \w     75.00 123.00   0.50   10.00    --  105.10 -82.00 -30.00   96
 16  \w     85.00 193.00   0.50   10.00    --  105.10  19.00-180.00  216
 17  \w     78.00 136.00   0.50   10.00    --  105.10 -82.00 -60.00  116
 18  \w     34.00  59.00   0.50   10.00    --  105.10 -82.00  60.00   50
 19  \w     87.00 112.00   0.50   10.00    --  105.10 -82.00  60.00   50
 20  \w     18.00 131.00   0.50   10.00    --  105.10 -77.00 150.00  226
 21  \w    143.00 186.00   0.50   10.00    --  105.10  82.00   0.00   86
 22  \w     88.00 113.00   0.50   10.00    --  105.10  82.00   0.00   50
 23  \w     84.00 109.00   0.50   10.00    --  105.10 -82.00-180.00   50
 24  \w     85.00 192.00   0.50   10.00    --  105.10  82.00 -60.00  214
 25  \w     51.00  76.00   0.50   10.00    --  105.10 -82.00 120.00   50
 26  \w     19.00 126.00   0.50   10.00    --  105.10 -82.00  30.00  214
 27  \w     43.00 127.00   0.50   10.00    --  105.10 -38.00   0.00  168
;
_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      -0.1562305000
_diffrn_orient_matrix_UB_12      0.0165853000
_diffrn_orient_matrix_UB_13      0.0002624000
_diffrn_orient_matrix_UB_21      -0.0230586000
_diffrn_orient_matrix_UB_22      -0.0328998000
_diffrn_orient_matrix_UB_23      0.0701998000
_diffrn_orient_matrix_UB_31      0.0664408000
_diffrn_orient_matrix_UB_32      0.0996152000
_diffrn_orient_matrix_UB_33      0.0651469000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29277
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.962
_diffrn_reflns_theta_min         2.747
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86630
_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    1.953
_exptl_crystal_description       needle
_exptl_crystal_F_000             1409
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         9849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0921P)^2^+1.6905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8365
_reflns_number_total             9849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01340d2.cif
_cod_data_source_block           180715a
_cod_depositor_comments
'Adding full bibliography for 7704312--7704315.cif.'
_cod_original_cell_volume        2390.32(7)
_cod_database_code               7704313
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOCuCl
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.904
_reflns_odcompleteness_completeness 99.72
_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) groups
2. Others
 Fixed Sof: H021(0.66667) H02C(0.33333) H02D(0.33333) C1(0.66667) H1A(0.66667)
 H1B(0.66667) C0AA(0.5) H0AB(0.5) H0AC(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 C22(0.33333) H22A(0.33333) H22B(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C01F(H01B,H01E), C01H(H01F,H01H), C01N(H01N,H01O), C01O(H01P,H01Q), C01S(H01T,
 H01U), C01U(H01W,H01X), C01X(H01,H), C01Y(H0AA,HA), C020(H02A,H02B), C021(H02C,
 H02D), C1(H1A,H1B), C0AA(H0AB,H0AC), C2(H2A,H2B), C22(H22A,H22B)
3.b Aromatic/amide H refined with riding coordinates:
 C015(H015), C016(H016), C019(H019), C01A(H01A), C01C(H01C), C01D(H01D),
 C01G(H01G), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M),
 C01P(H01R), C01R(H01S), C01T(H01V), C01V(H01Y), C01W(H01Z), C01Z(H1AA),
 C021(H021)
;
_shelx_res_checksum              62921
_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 1.871
_oxdiff_exptl_absorpt_empirical_full_min 0.737