Base induced C–CN bond cleavage at room temperature: a convenient method for the activation of acetonitrile
Zhang, Xiaofeng; Zhang, Zilong; Xiang, Shiqun; Zhu, Yingzu; Chen, Changneng; Huang, Deguang; Inorganic Chemistry Frontiers 6 (2019) 1135–; doi:10.1039/C8QI01258J

data_4349972
_publ_section_title
;
 Base induced C--CN bond cleavage at room temperature: a convenient method
 for the activation of acetonitrile
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1135
_journal_paper_doi               10.1039/C8QI01258J
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C54 H35 Cu2 N6 O5, C8 H20 N, C3 H7 N O'
_chemical_formula_sum            'C65 H62 Cu2 N8 O6'
_chemical_formula_weight         1178.31
_chemical_name_common            '[Cu(NNN-Naph)-OH-Cu(NNN-Naph)](Et4N).DMF'
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-12-11 deposited with the CCDC.	2019-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.409(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.5931(5)
_cell_length_b                   12.2058(5)
_cell_length_c                   16.6043(5)
_cell_measurement_reflns_used    3223
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.7540
_cell_measurement_theta_min      3.8320
_cell_volume                     2944.40(18)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5641
_diffrn_reflns_theta_full        71.88
_diffrn_reflns_theta_max         71.88
_diffrn_reflns_theta_min         3.86
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  0.7186
_exptl_absorpt_correction_T_min  0.5795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies,Version 1.171.36.28 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         4158
_refine_ls_number_restraints     1040
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+2.5270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1517
_refine_special_details
; 
The two naphthalin rings and the Et4N+ cation molecule of this structure was treated
as disordered models with occupancies of 55/45, respectively. The occupancy of DMF 
set to 50% according to its symmetrical location in the model, which offers the other 
50% occupancy after using 'grow' command. The distance of 2.37 angstrom between the 
original half DMF molecule and the other symmetrical half DMF also indicates that these
two parts are NOT independent units.   
;
_reflns_number_gt                4086
_reflns_number_total             4158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qi01258j2.cif
_cod_data_source_block           Complex9
_cod_original_cell_volume        2944.41(17)
_cod_original_sg_symbol_H-M      'I 2 '
_cod_database_code               4349972