Metal‒organic and supramolecular lead(ii) networks assembled from isomeric nicotinoylhydrazone blocks: the effects of ligand geometry and counter-ion on topology and supramolecular assembly
Mahmoudi, Ghodrat; Bauzá, Antonio; Frontera, Antonio; Garczarek, Piotr; Stilinović, Vladimir; Kirillov, Alexander M.; Kennedy, Alan; Ruiz-Pérez, Catalina; CrystEngComm 18 (2016) 5375–; doi:10.1039/C6CE00900J

data_7226173
_publ_section_title
;
 Metal--organic and supramolecular lead(ii) networks assembled from
 isomeric nicotinoylhydrazone blocks: the effects of ligand geometry and
 counter-ion on topology and supramolecular assembly
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5375
_journal_paper_doi               10.1039/C6CE00900J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C15 H12 N6 O Pb S2'
_chemical_formula_weight         563.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-19 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                87.356(7)
_cell_angle_beta                 87.566(5)
_cell_angle_gamma                82.906(5)
_cell_formula_units_Z            2
_cell_length_a                   8.6135(4)
_cell_length_b                   9.3532(7)
_cell_length_c                   11.1952(10)
_cell_measurement_reflns_used    8887
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      2.61
_cell_measurement_theta_min      28.60
_cell_volume                     893.46(11)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR92, J. Appl. Cryst. 26, 343-350, (1993)')'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8887
_diffrn_reflns_theta_full        28.60
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         2.91
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    9.691
_exptl_absorpt_correction_T_max  0.2090
_exptl_absorpt_correction_T_min  0.1872
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.901
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1.6668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                4115
_reflns_number_total             4459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00900j2.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7226173