Copper(II)-hydroxide facilitated C-C bond formation: the carboxamido pyridine system <i>versus</i> the methylimino pyridine system.
Li, Yinghua; Fan, Weibin; Zhang, Zilong; Xie, Xingkun; Xiang, Shiqun; Huang, Deguang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12189–12196; doi:10.1039/d0dt02288h

data_7705180
_publ_section_title
;
 Copper(II)-hydroxide facilitated C-C bond formation: the carboxamido
 pyridine system <i>versus</i> the methylimino pyridine system.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12189
_journal_page_last               12196
_journal_paper_doi               10.1039/d0dt02288h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C48 H46 Cu N6 O2, C4 H12 N, 1.5(C4 H10 O), 0.5(H2 O)'
_chemical_formula_sum            'C58 H74 Cu N7 O4'
_chemical_formula_weight         996.78
_chemical_name_common            '[[Cu(dimer-ligand)](Me4N) (Et2O)1.5 (H2O)0.5'
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-08-12 deposited with the CCDC.	2020-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                82.653(4)
_cell_angle_beta                 68.845(3)
_cell_angle_gamma                68.250(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7226(11)
_cell_length_b                   15.0739(14)
_cell_length_c                   16.6986(15)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.62
_cell_volume                     2773.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            106412
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.616
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         10899
_refine_ls_number_restraints     1916
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1328P)^2^+0.3470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.2307
_refine_special_details
;
The data used for structure solution was derived from a poor quality crystal.
Many atoms were treated as disordered model with their occupancies refined
freely. The final refinement of structure model gave the occupancies of main
structure and Me4N cation as 0.59 and 0.41. The two Et2O molecules were
treated as disordered models with occupancies of 0.59/0.41 and 0.52/0.48,
respectively. The bond lengths, bond angles and the temperature factors of
those disordered atoms were restrained by using commands of DFIX and DELU &
SIMU, except for the disordered copper ion which was refined freely.
The hydrogen atoms were added geometrically except for those for water
molecule on which the two hydrogen atoms were added from Fourier Maps and set
to point to the hydrogen acceptors of oxygen and nitrogen atoms on the ligand.
;
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6679
_reflns_number_total             10899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02288h2.cif
_cod_data_source_block           Complex12
_cod_depositor_comments
'Adding full bibliography for 7705173--7705180.cif.'
_cod_database_code               7705180
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.849
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              37849