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_4516549
_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         '(C8 H12 Cl4 Cu2 O10), 2.5 (H2 O)'
_chemical_formula_sum            'C8 H17 Cl4 Cu2 O12.5'
_chemical_formula_weight         582.095
_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                65.155(3)
_cell_angle_beta                 76.631(2)
_cell_angle_gamma                88.938(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3022(3)
_cell_length_b                   13.1824(4)
_cell_length_c                   15.4119(4)
_cell_measurement_reflns_used    22387
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.7730
_cell_measurement_theta_min      1.7220
_cell_volume                     2019.18(11)
_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                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source, Pilatus 200/300K'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55602
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.094
_diffrn_reflns_theta_min         1.709
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.690
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.498
_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    1.915
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         13028
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.8720P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9545
_reflns_number_total             13028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b01365_si_001.cif
_cod_data_source_block           1
_cod_database_code               4516549
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.454
_shelx_estimated_absorpt_t_max   0.773
_shelxl_version_number           2014-7
_shelx_res_checksum              69181
_shelx_hkl_checksum              16408