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_7702488
_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         'C16 H16 Cu N4 O5 S, 3(H2 O)'
_chemical_formula_structural     '[Cu(SO4)(tpm)(H2O)].3H2O'
_chemical_formula_sum            'C16 H22 Cu N4 O8 S'
_chemical_formula_weight         493.98
_chemical_name_common            'Complex 1'
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.729(3)
_cell_length_b                   8.0736(9)
_cell_length_c                   17.869(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1980.6(5)
_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  0.019
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2858
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.235
_exptl_absorpt_correction_T_min  0.125
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            turquoise
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       'thick plates'
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.850
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment
;
 Hydrogen atoms on the pyridyl rings were included in idealised positions;
 the two amino hydrogens were located in a difference map and refined with
 geometrical constraints.  The isotropic factors of all hydrogen atoms were
 allowed to refine freely. 
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         2457
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_obs          0.0537
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0909P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1389
_refine_ls_wR_factor_obs         0.1279
_reflns_number_observed          1963
_reflns_number_total             2457
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b008476j.txt
_cod_data_source_block           marcus11
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0909P)^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^)+(0.0909P)^2^] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_cell_volume        1980.7(5)
_cod_original_sg_symbol_H-M      'P n a 21 (no. 33)'
_cod_database_code               7702488