Copper complexes of the functionalised tripodal ligand tris(2-pyridyl)methylamine and its derivatives †
Arnold, Phillip J.; Davies, Sian C.; Dilworth, Jonathan R.; Durrant, Marcus C.; Griffiths, D. Vaughan; Hughes, David L.; Richards, Raymond L.; Sharpe, Philip C.; Journal of the Chemical Society, Dalton Transactions  (2001) 736–; doi:10.1039/b008476j

data_7702494
_publ_section_title
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 Copper complexes of the functionalised tripodal ligand
 tris(2-pyridyl)methylamine and its derivatives&#x200A;&#x2020;
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_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              736
_journal_paper_doi               10.1039/b008476j
_journal_year                    2001
_chemical_formula_moiety
'2(C16 H20 N4 O3 Zn), H12 O6 Zn, 3(S O4), 3(H2 O)'
_chemical_formula_structural     '[Zn(tpm)(H2O)3]2 [Zn(H2O)6] (SO4)3 .3H2O'
_chemical_formula_sum            'C32 H58 N8 O27 S3 Zn3'
_chemical_formula_weight         1279.15
_chemical_name_common            'Complex 20'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           'Monoclinic, twinned'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.652(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5362(15)
_cell_length_b                   13.789(2)
_cell_length_c                   22.407(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     4748.7(10)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'CAD4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; \w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11830
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.736
_exptl_absorpt_correction_T_max  0.19
_exptl_absorpt_correction_T_min  0.16
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_hydrogen_treatment
;
 Hydrogen atoms on the pyridyl rings were included in idealised positions and,
 in the refinement, all parameters were set to ride on those of the parent C 
 atoms.  Some of the H atoms of the amine groups and the water molecules were 
 located from difference maps and were refined with constrained O-H or N-H 
 distances.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         11434
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.078
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_obs          0.0436
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0677P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1154
_refine_ls_wR_factor_obs         0.1045
_reflns_number_observed          9411
_reflns_number_total             11434
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b008476j.txt
_cod_data_source_block           philip1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0677P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. A new data item '_refine_ls_weighting_details' was created
with the value set to 'w=1/[\s^2^(Fo^2^)+(0.0677P)^2^] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4748.6(9)
_cod_original_sg_symbol_H-M      'P 21/a (equiv. to no. 14)'
_cod_database_code               7702494