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_7030933
_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
'2(C42 H45 Cl4 N17 O19 Pb2), C4 H10 O, 4(C2 H3 N), 2(O)'
_chemical_formula_sum            'C96 H112 Cl8 N38 O41 Pb4'
_chemical_formula_weight         3566.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.000
_cell_angle_beta                 109.239(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   29.752(3)
_cell_length_b                   10.5359(9)
_cell_length_c                   44.383(4)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.38
_cell_volume                     13135(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            43553
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.368
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             6984
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.555
_refine_diff_density_min         -3.170
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         12429
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0340P)^2^+424.2833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                10521
_reflns_number_total             12429
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt53559b2.cif
_cod_data_source_block           3(sdjh878)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        13135(4)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               7030933