Reaction of Copper(II) Chloroacetate with Pyrazole. Synthesis of a One-Dimensional Coordination Polymer and Unexpected Dehydrochlorination Reaction
Carlotto, Silvia; Casarin, Maurizio; Lanza, Arianna; Nestola, Fabrizio; Pandolfo, Luciano; Pettinari, Claudio; Scatena, Rebecca; Crystal Growth & Design 15 (2015) 5910–; doi:10.1021/acs.cgd.5b01365

data_4516548
_publ_section_title
;
 Reaction of Copper(II) Chloroacetate with Pyrazole. Synthesis of a
 One-Dimensional Coordination Polymer and Unexpected Dehydrochlorination
 Reaction
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5910
_journal_paper_doi               10.1021/acs.cgd.5b01365
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C17 H20 Cl Cu3 N10 O3, Cl'
_chemical_formula_sum            'C17 H20 Cl2 Cu3 N10 O3'
_chemical_formula_weight         673.95
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                78.816(8)
_cell_angle_beta                 78.074(8)
_cell_angle_gamma                68.557(9)
_cell_formula_units_Z            2
_cell_length_a                   8.8168(9)
_cell_length_b                   8.9397(9)
_cell_length_c                   16.8959(16)
_cell_measurement_reflns_used    5036
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.7630
_cell_measurement_theta_min      2.4440
_cell_volume                     1202.5(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_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      296(2)
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Pilatus 200/300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17358
_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         25.998
_diffrn_reflns_theta_min         2.469
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.894
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       prism
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.1440
_exptl_crystal_size_mid          0.1011
_exptl_crystal_size_min          0.0774
_refine_diff_density_max         1.762
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4713
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1086P)^2^+7.6879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2122
_refine_ls_wR_factor_ref         0.2324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3381
_reflns_number_total             4713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b01365_si_004.cif
_cod_data_source_block           4
_cod_depositor_comments
;

2021-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C34 H40 Cl4 Cu6 N20 O6'
_cod_original_formula_weight         1347.90
_cod_original_formula_moiety         'C34 H40 Cl2 Cu6 N20 O6, 2(Cl)'
_cod_original_formula_units_Z            1
_cod_database_code               4516548
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              24538
_shelx_hkl_checksum              94861