Copper(ii) facilitated decarboxylation for the construction of pyridyl–pyrazole skeletons
Xiang, Shiqun; Zhang, Xiaofeng; Chen, Hui; Li, Yinghua; Fan, Weibin; Huang, Deguang; Inorganic Chemistry Frontiers 6 (2019) 2359–; doi:10.1039/C9QI00599D

data_4350073
_publ_section_title
;
 Copper(ii) facilitated decarboxylation for the construction of
 pyridyl--pyrazole skeletons
;
_journal_issue                   9
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2359
_journal_paper_doi               10.1039/C9QI00599D
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C10 H2 Cu N4 O8, 4(C8 H20 N), 10(H2 O)'
_chemical_formula_sum            'C42 H102 Cu N8 O18'
_chemical_formula_weight         1070.86
_chemical_name_common            (Et4N)4[Cu(pdc)2](H2O)10
_chemical_name_systematic        (Et4N)4[Cu(pdc)2](H2O)10
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-09-05 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2825(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.6716(4)
_cell_length_b                   7.91640(15)
_cell_length_c                   32.9340(5)
_cell_measurement_reflns_used    6183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.8550
_cell_measurement_theta_min      4.0750
_cell_volume                     5640.92(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega 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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            10445
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.9556
_exptl_absorpt_correction_T_min  0.8378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            needle
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       purple
_exptl_crystal_F_000             2332
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+2.6365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                4763
_reflns_number_total             5324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9qi00599d2.cif
_cod_data_source_block           full_CCDC3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4350073