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_7704314
_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 H42 Ag3 Cu3 N20 O6, N O3'
_chemical_formula_sum            'C36 H42 Ag3 Cu3 N21 O9'
_chemical_formula_weight         1427.13
_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
_audit_creation_date             2020-02-04
_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                109.865(4)
_cell_angle_beta                 96.933(4)
_cell_angle_gamma                102.870(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4794(6)
_cell_length_b                   15.6237(8)
_cell_length_c                   17.3463(6)
_cell_measurement_reflns_used    11000
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      75.8960
_cell_measurement_theta_min      3.2890
_cell_volume                     2300.8(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.945
_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      0.00  25.00   0.50    0.50    --    0.00  14.00  44.00   50
  2  \w    -65.00  -8.00   0.50    0.50    --    0.00 -14.00-127.00  114
  3  \w     15.00 143.00   0.50    1.70    --  102.90 -14.00-127.00  256
  4  \w    127.00 157.00   0.50    1.70    --  102.90  14.00  44.00   60
  5  \w    -31.00  48.00   0.50    0.50    --    0.00  77.00  90.00  158
  6  \w    -25.00  82.00   0.50    0.50    --    0.00  57.00  30.00  214
  7  \w    -34.00  12.00   0.50    0.50    --    0.00  82.00   0.00   92
  8  \w    -37.00   6.00   0.50    0.50    --    0.00 -82.00  60.00   86
  9  \w     73.00 100.00   0.50    1.70    --  102.90 -82.00 -90.00   54
 10  \w     70.00 191.00   0.50    1.70    --  102.90  19.00-120.00  242
 11  \w    101.00 127.00   0.50    1.70    --  102.90 -82.00 150.00   52
 12  \w     81.00 108.00   0.50    1.70    --  102.90 -82.00  60.00   54
 13  \w    163.00 191.00   0.50    1.70    --  102.90  82.00-180.00   56
 14  \w     29.00 133.00   0.50    1.70    --  102.90 -82.00  30.00  208
 15  \w     91.00 121.00   0.50    1.70    --  102.90  19.00-150.00   60
 16  \w     24.00 137.00   0.50    1.70    --  102.90 -82.00 120.00  226
 17  \w    138.00 192.00   0.50    1.70    --  102.90  19.00 -60.00  108
 18  \w     93.00 120.00   0.50    1.70    --  102.90 -82.00-180.00   54
 19  \w     63.00  88.00   0.50    1.70    --  102.90 -82.00-180.00   50
 20  \w     70.00 112.00   0.50    1.70    --  102.90  19.00 -60.00   84
 21  \w    113.00 138.00   0.50    1.70    --  102.90  82.00-180.00   50
 22  \w     44.00 121.00   0.50    1.70    --  102.90 -82.00 -60.00  154
 23  \w     25.00 128.00   0.50    1.70    --  102.90 -57.00 -90.00  206
 24  \w     25.00 132.00   0.50    1.70    --  102.90 -82.00  90.00  214
;
_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      0.0623823000
_diffrn_orient_matrix_UB_12      0.1059089000
_diffrn_orient_matrix_UB_13      0.0163079000
_diffrn_orient_matrix_UB_21      0.1507226000
_diffrn_orient_matrix_UB_22      -0.0160878000
_diffrn_orient_matrix_UB_23      -0.0146495000
_diffrn_orient_matrix_UB_31      -0.0501812000
_diffrn_orient_matrix_UB_32      -0.0216733000
_diffrn_orient_matrix_UB_33      -0.0941568000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22359
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.073
_diffrn_reflns_theta_min         3.135
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    12.226
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21488
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_description       needle
_exptl_crystal_F_000             1410
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.990
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         9200
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0767
_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^)+(0.1582P)^2^+8.6304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2203
_refine_ls_wR_factor_ref         0.2332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8051
_reflns_number_total             9200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01340d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7704312--7704315.cif.'
_cod_database_code               7704314
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.792
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00U(0.036) H00W(0.033) H00Y(0.039) H011(0.039) H012(0.038)
 H013(0.041) H01A(0.05) H01B(0.05) H016(0.037) H017(0.042) H019(0.039)
 H01C(0.043) H01D(0.049) H01E(0.049) H01F(0.04) H01G(0.047) H01H(0.045)
 H01I(0.045) H01J(0.045) H01K(0.045) H01L(0.046) H01M(0.044) H01N(0.044)
 H01O(0.045) H01P(0.045) H01Q(0.042) H01R(0.04) H01S(0.04) H01T(0.046)
 H01U(0.046) H01V(0.054) H01W(0.051) H01X(0.054) H01Y(0.055) H01Z(0.044)
 H(0.044) H01(0.037) HA(0.037) H0AA(0.044) HB(0.044) H02A(0.043) H02B(0.043)
 H1A(0.033) H1B(0.033) H2A(0.029) H2B(0.029) H4A(0.051) H4B(0.051) H5A(0.041)
 H5B(0.041)
 Fixed X: H00U(0.884369) H00W(0.724622) H00Y(0.926735) H011(1.251757)
 H012(0.82833) H013(0.43857) H01A(1.234593) H01B(1.183516) H016(1.018545)
 H017(1.329513) H019(0.691244) H01C(0.319691) H01D(0.961915) H01E(0.985789)
 H01F(0.831103) H01G(0.439689) H01H(0.559422) H01I(0.572637) H01J(0.937926)
 H01K(0.813652) H01L(0.578159) H01M(1.360465) H01N(1.277506) H01O(0.806227)
 H01P(0.818198) H01Q(0.487625) H01R(0.807227) H01S(0.656111) H01T(1.087593)
 H01U(0.920578) H01V(0.221839) H01W(0.354035) H01X(0.442797) H01Y(0.173034)
 H01Z(0.018355) H(0.12438) H01(0.221334) HA(0.329595) H0AA(0.057811)
 HB(0.072767) H02A(0.33277) H02B(0.261434) H1A(0.037419) H1B(-0.017905)
 H2A(0.373906) H2B(0.401939) H4A(0.17057) H4B(0.03882) H5A(0.156456)
 H5B(0.193309)
 Fixed Y: H00U(0.290909) H00W(0.589853) H00Y(0.792818) H011(0.379089)
 H012(0.216182) H013(0.932648) H01A(-0.104784) H01B(-0.035644) H016(0.633856)
 H017(0.196952) H019(-0.03237) H01C(0.794245) H01D(-0.062572) H01E(-0.162727)
 H01F(-0.131088) H01G(0.312536) H01H(0.977711) H01I(1.029846) H01J(1.010152)
 H01K(1.045972) H01L(0.183248) H01M(0.055588) H01N(0.003806) H01O(1.085467)
 H01P(0.986663) H01Q(0.598978) H01R(0.892071) H01S(0.893194) H01T(-0.130843)
 H01U(-0.184283) H01V(0.66173) H01W(0.435872) H01X(0.26941) H01Y(0.624572)
 H01Z(0.477666) H(0.496879) H01(0.606813) HA(0.544899) H0AA(0.34033)
 HB(0.344928) H02A(0.409336) H02B(0.299176) H1A(0.373878) H1B(0.425797)
 H2A(0.490396) H2B(0.413742) H4A(0.571226) H4B(0.537422) H5A(0.340614)
 H5B(0.444597)
 Fixed Z: H00U(0.422277) H00W(0.581857) H00Y(0.891957) H011(0.593931)
 H012(0.263945) H013(0.664982) H01A(0.427242) H01B(0.49997) H016(0.780017)
 H017(0.52754) H019(0.076987) H01C(0.490415) H01D(0.417528) H01E(0.40103)
 H01F(0.171891) H01G(0.090916) H01H(0.852069) H01I(0.789069) H01J(0.923027)
 H01K(0.964963) H01L(-0.109559) H01M(0.458223) H01N(0.363961) H01O(0.849769)
 H01P(0.792341) H01Q(0.524732) H01R(0.960809) H01S(0.913884) H01T(0.279931)
 H01U(0.26855) H01V(0.192277) H01W(0.170024) H01X(-0.21384) H01Y(0.009938)
 H01Z(-0.197064) H(-0.2555) H01(-0.119817) HA(-0.146712) H0AA(-0.295558) HB(-
 0.203349) H02A(-0.250911) H02B(-0.28479) H1A(-0.180431) H1B(-0.235953) H2A(-
 0.167898) H2B(-0.246161) H4A(-0.139939) H4B(-0.100586) H5A(-0.288921) H5B(-
 0.285036)
;
_shelx_res_checksum              62160
_shelx_fab_checksum              15686
_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 4.269
_oxdiff_exptl_absorpt_empirical_full_min 0.303