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_7030934
_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
'C54 H54 Cu3 F12 N18 O17 S4, 2(C F3 O3 S), 2(C2 H3 N), H2 O'
_chemical_formula_sum            'C60 H62 Cu3 F18 N20 O24 S6'
_chemical_formula_weight         2172.28
_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                113.9013(11)
_cell_angle_beta                 92.2282(9)
_cell_angle_gamma                105.8198(11)
_cell_formula_units_Z            2.00000
_cell_length_a                   11.93796(15)
_cell_length_b                   18.6842(2)
_cell_length_c                   21.6335(2)
_cell_measurement_reflns_used    47395
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.3080
_cell_measurement_theta_min      4.1400
_cell_volume                     4182.87(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      100.01(10)
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            96122
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    3.413
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2198
_exptl_crystal_size_max          0.3892
_exptl_crystal_size_mid          0.1447
_exptl_crystal_size_min          0.0735
_refine_diff_density_max         2.286
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1206
_refine_ls_number_reflns         14909
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0838
_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^)+(0.1571P)^2^+10.6915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2397
_refine_ls_wR_factor_ref         0.2487
_reflns_number_gt                13185
_reflns_number_total             14909
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt53559b2.cif
_cod_data_source_block           4(dh1211)
_cod_database_code               7030934