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_7702490
_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         'C32 H28 Cu N8, 2(B F4), C3 H6 O'
_chemical_formula_structural     '[Cu(tpm)2](BF4)2.Me2CO'
_chemical_formula_sum            'C35 H34 B2 Cu F8 N8 O'
_chemical_formula_weight         819.9
_chemical_name_common            'Complex 6'
_space_group_IT_number           15
_space_group_name_Hall           '-A 2ya'
_space_group_name_H-M_alt        'A 1 2/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'A 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'automated Patterson'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.259(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8308(14)
_cell_length_b                   10.8103(12)
_cell_length_c                   22.990(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     3666.7(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  0.016
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            3588
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        2.7
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       plates
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_hydrogen_treatment
;
 The cation hydrogen atoms were included in idealised positions and then 
 allowed to refine freely.  The solvent H atoms were input in idealised 
 positions and set to ride on the parent carbon atoms.  Isotropic thermal
 parameters of all H atoms were refined freely.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         3211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_obs          0.0357
_refine_ls_shift/esd_max         0.046
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+3.9788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0857
_refine_ls_wR_factor_obs         0.0745
_reflns_number_observed          2284
_reflns_number_total             3211
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b008476j.txt
_cod_data_source_block           marcus15
_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^)+(0.0163P)^2^+3.9788P] 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^)+(0.0163P)^2^+3.9788P] 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        3666.6(6)
_cod_original_sg_symbol_H-M      'A 2/a (equiv. to no. 15)'
_cod_database_code               7702490