Synergic effect of copper-based metal‒organic frameworks for highly efficient C‒H activation of amidines
Xu, Fen; Kang, Wei-Fen; Wang, Xiao-Ning; Kou, Hao-Dong; Jin, Zhen; Liu, Chun-Sen; RSC Advances 7 (2017) 51658–; doi:10.1039/C7RA10682C

data_7229533
_publ_section_title
;
 Synergic effect of copper-based metal--organic frameworks for highly
 efficient C--H activation of amidines
;
_journal_issue                   81
_journal_name_full               'RSC Advances'
_journal_page_first              51658
_journal_paper_doi               10.1039/C7RA10682C
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C56 H34 Cu2 N6 O14'
_chemical_formula_sum            'C56 H34 Cu2 N6 O14'
_chemical_formula_weight         1141.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-03 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                111.443(4)
_cell_angle_beta                 91.846(3)
_cell_angle_gamma                95.794(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1088(4)
_cell_length_b                   16.9597(8)
_cell_length_c                   19.1362(4)
_cell_measurement_reflns_used    9059
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.9810
_cell_measurement_theta_min      4.5590
_cell_volume                     3629.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3031
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -67.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2955   57.0000   60.0000 99

  2 omega   89.00  115.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2955   38.0000  -60.0000 26

  3 omega   82.00  169.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410   30.0000    0.0000 87

  4 omega  125.00  172.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  125.0000 -120.0000 47

  5 omega  110.00  170.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410   77.0000 -150.0000 60

  6 omega   88.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410   45.0000  -90.0000 88

  7 omega   66.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000    0.0000 32

  8 omega   49.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -95.0000   30.0000 57

  9 omega   45.00  116.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410 -125.0000    0.0000 71

 10 omega   37.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000   90.0000 52

 11 omega   40.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -77.0000  150.0000 100

 12 omega   32.00   84.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000  -30.0000 52

 13 omega   34.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000  -90.0000 64

 14 omega   68.00   97.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000 -150.0000 29

 15 omega   89.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410 -125.0000 -180.0000 32

 16 omega   20.00   81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2955  -99.0000 -150.0000 61

 17 omega  -50.00   34.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2955   38.0000 -150.0000 84

 18 omega   15.00   58.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2955  -99.0000  120.0000 43

 19 omega   33.00   87.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000  150.0000 54

 20 omega -108.00  -16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2955  -57.0000  -90.0000 92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0098172000
_diffrn_orient_matrix_UB_12      0.0973200000
_diffrn_orient_matrix_UB_13      0.0426071000
_diffrn_orient_matrix_UB_21      -0.0329491000
_diffrn_orient_matrix_UB_22      -0.0139299000
_diffrn_orient_matrix_UB_23      0.0720991000
_diffrn_orient_matrix_UB_31      0.1235432000
_diffrn_orient_matrix_UB_32      0.0009184000
_diffrn_orient_matrix_UB_33      0.0225636000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24542
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.679
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_F_000             1164
_platon_squeeze_details
;
;
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         12970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0786
_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^)+(0.1790P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2250
_refine_ls_wR_factor_ref         0.2442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9585
_reflns_number_total             12970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra10682c2.cif
_cod_data_source_block           20160120wxn-1
_cod_database_code               7229533
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O N Cu'
_chemical_oxdiff_usercomment     1591
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C35(H35), C39(H39), C37(H37), C47(H47), C41(H41), C42(H42), C33(H33),
 C32(H32), C29(H29), C44(H44), C45(H45), C53(H53), C46(H46), C30(H30), C52(H52),
  C49(H49), C50(H50), C7(H7), C11(H11), C6(H6), C13(H13), C9(H9), C22(H22),
 C24(H24), C21(H21), C3(H3), C25(H25), C19(H19), C4(H4), C18(H18), C16(H16),
 C15(H15), C56(H56), C55(H55)
;
_olex2_submission_special_instructions 'No special instructions were received'