Tetratopic pyrimidine-hydrazone ligands modified with terminal hydroxymethyl and acryloyl arms and their Pb(ii), Zn(ii), Cu(ii) and Ag(i) complexes.
Hutchinson, Daniel J.; Hanton, Lyall R.; Moratti, Stephen C.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 8205–8218; doi:10.1039/c3dt53559b

data_7030931
_publ_section_title
;
 Tetratopic pyrimidine-hydrazone ligands modified with terminal
 hydroxymethyl and acryloyl arms and their Pb(ii), Zn(ii), Cu(ii) and
 Ag(i) complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8205
_journal_page_last               8218
_journal_paper_doi               10.1039/c3dt53559b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C41 H49 Cl7 N17 O34 Pb4, 3(C H3 N O2), (Cl O4)'
_chemical_formula_sum            'C44 H58 Cl8 N20 O44 Pb4'
_chemical_formula_weight         2683.46
_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
_cell_angle_alpha                102.491(4)
_cell_angle_beta                 93.675(4)
_cell_angle_gamma                104.479(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2296(10)
_cell_length_b                   17.3147(18)
_cell_length_c                   25.755(3)
_cell_measurement_reflns_used    7074
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      21.21
_cell_measurement_theta_min      2.45
_cell_volume                     3860.3(7)
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEXII 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     0.71069
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39972
_diffrn_reflns_theta_full        21.24
_diffrn_reflns_theta_max         21.24
_diffrn_reflns_theta_min         1.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.087
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.569
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         8364
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+132.8490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1390
_reflns_number_gt                7006
_reflns_number_total             8364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53559b2.cif
_cod_data_source_block           1(djh558)
_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/rss-feeds/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7030931