Coordination behaviour of new dipyridylpyrazole ligands towards ZnCl2and PdCl2fragments. Crystalline structural characterization and multinuclear NMR studies as evidence of linkage and conformational isomers
Soria, Lorena; Ovejero, Paloma; Cano, Mercedes; Heras, José Vicente; Torres, M. Rosario; Claramunt, Rosa; Cornago, Pilar; RSC Adv. 4 (2014) 9383–; doi:10.1039/C3RA45821K

data_7239404
_publ_section_title
;
 Coordination behaviour of new dipyridylpyrazole ligands towards ZnCl2and
 PdCl2fragments. Crystalline structural characterization and multinuclear
 NMR studies as evidence of linkage and conformational isomers
;
_journal_issue                   18
_journal_name_full               'RSC Adv.'
_journal_page_first              9383
_journal_paper_doi               10.1039/C3RA45821K
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C20 H16 Cl2 N4 O Zn'
_chemical_formula_weight         464.64
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.413(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.105(3)
_cell_length_b                   21.483(5)
_cell_length_c                   8.0777(19)
_cell_measurement_reflns_used    1428
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.17
_cell_measurement_theta_min      2.76
_cell_volume                     2212.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_av_sigmaI/netI    0.2220
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16529
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       thin
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;

 The final refinement show high values of residual non-modelled 
 electronic density. Therefore, the Squeeze program was used to 
 remove its contribution to the overal intensity data. An 
 improvement was observed in all refinement parameters and residual
 when this procedure is applied.   
;
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1856
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2039
_reflns_number_gt                1322
_reflns_number_total             3876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra45821k.txt
_cod_data_source_block           C20H16Cl2N4O1Zn1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7239404