Green carbon-carbon homocoupling of terminal alkynes by a silica supported Cu(II)-hydrazone coordination compound.
Heydari, Neda; Bikas, Rahman; Siczek, Milosz; Lis, Tadeusz; Dalton transactions (Cambridge, England : 2003) 52 (2023) 421–433; doi:10.1039/d2dt03054c

data_7711848
_publ_section_title
;
 Green carbon-carbon homocoupling of terminal alkynes by a silica
 supported Cu(II)-hydrazone coordination compound.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              421
_journal_page_last               433
_journal_paper_doi               10.1039/d2dt03054c
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C16 H18 Cu N4 O7, C H4 O'
_chemical_formula_sum            'C17 H22 Cu N4 O8'
_chemical_formula_weight         473.92
_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-2013
_audit_update_record
;
2022-09-19 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                98.42(5)
_cell_angle_beta                 105.98(5)
_cell_angle_gamma                107.55(5)
_cell_formula_units_Z            2
_cell_length_a                   7.814(2)
_cell_length_b                   11.098(3)
_cell_length_c                   12.616(4)
_cell_measurement_reflns_used    4766
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.8
_cell_volume                     970.9(7)
_computing_cell_refinement       'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_data_collection       'CrysAlis CCD; Oxford-Diffraction Poland, 2003'
_computing_data_reduction        'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type
;
Kuma KM4 kappa-geometry diffractometer with a CCD detector
;
_diffrn_measurement_method       w/
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9665
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.835
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1000P)^2^+0.6156P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3888
_reflns_number_total             4428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03054c2.cif
_cod_data_source_block           pa102a
_cod_depositor_comments
'Adding full bibliography for 7711848--7711849.cif.'
_cod_original_cell_volume        970.9(6)
_cod_database_code               7711848
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.891
_shelxl_version_number           2013-2
_shelx_res_checksum              33970