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_7030935
_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
'C80 H84 Ag2 N32 O4, 2(C F3 O3 S), C2 H3 N, H2 O'
_chemical_formula_sum            'C84 H89 Ag2 F6 N33 O11 S2'
_chemical_formula_weight         2130.77
_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                90.879(8)
_cell_angle_beta                 104.340(8)
_cell_angle_gamma                99.074(8)
_cell_formula_units_Z            2
_cell_length_a                   15.957(3)
_cell_length_b                   16.872(3)
_cell_length_c                   17.655(3)
_cell_measurement_reflns_used    7143
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      18.82
_cell_measurement_theta_min      2.45
_cell_volume                     4540.1(14)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22229
_diffrn_reflns_theta_full        18.82
_diffrn_reflns_theta_max         18.82
_diffrn_reflns_theta_min         1.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1327
_refine_ls_number_reflns         7056
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+60.8872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                6174
_reflns_number_total             7056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53559b2.cif
_cod_data_source_block           5(djh466)
_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               7030935