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_7702493
_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         'C26 H30 CU2 N6 O8 S4, 3(O H2)'
_chemical_formula_structural     '[{Cu(mde)(SO4)-O,O'}2].3(H2O)'
_chemical_formula_sum            'C26 H36 Cu2 N6 O11 S4'
_chemical_formula_weight         863.9
_chemical_name_common            'Complex 18'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.24(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1541(14)
_cell_length_b                   13.264(2)
_cell_length_c                   14.255(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1723.6(6)
_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  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            '4859 (to theta of 26.0)'
_diffrn_reflns_theta_max         '24.00 (collected to theta of 26.0)'
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        4.93
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.54
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'Bright blue'
_exptl_crystal_density_diffrn    1.67
_exptl_crystal_description       'irregular octahedra'
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_hydrogen_treatment
;
 Coordinates of the complex hydrogens were located in idealised postions and
 set to ride on the parent atoms.  Those of one of the two solvent water
 hydrogens were geometrically constrained.  Hydrogens were not included in the
 second water molecule.  All isotropic thermal displacement parameters were 
 set to be 1.2 x Ueq of the parent atoms.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2712
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_obs          0.0489
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1176
_refine_ls_wR_factor_obs         0.0976
_reflns_number_observed          '1798 (2015 to theta of 26.0)'
_reflns_number_total             '2712 (3374 to theta of 26.0)'
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b008476j.txt
_cod_data_source_block           marcus23
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0467P)^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^)+(0.0467P)^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        1723.7(6)
_cod_original_sg_symbol_H-M      'P 21 / n  (equiv. to no. 14)'
_cod_database_code               7702493