Complexes of the tripodal nitrilotrimethylenetrisphosphonic (H6L) and P,P′,P ″-triphenylnitrilotrimethylenetrisphosphinic (H3L°) acids with the copper(II) ion. Synthesis and characterization of [Hpy][Cu(H3L)(H2O)] and [Cu(HL°)(py)]2·2Me2CO†
Cecconi, Franco; Ghilardi, Carlo A.; Lorenzo Luis, Pablo A.; Midollini, Stefano; Orlandini, Annabella; Dakternieks, Dainis; Duthie, Andrew; Dominguez, Sixto; Berti, Elisabetta; Vacca, Alberto; Journal of the Chemical Society, Dalton Transactions  (2001) 211–; doi:10.1039/b004576o

data_7702438
_publ_section_title
;
 Complexes of the tripodal nitrilotrimethylenetrisphosphonic (H6L) and
 P,P&#x2032;,P&#x200A;&#x2033;-triphenylnitrilotrimethylenetrisphosphinic
 (H3L\%) acids with the copper(II) ion. Synthesis and characterization of
 [Hpy][Cu(H3L)(H2O)] and [Cu(HL\%)(py)]2&#x00B7;2Me2CO&#x2020;
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              211
_journal_paper_doi               10.1039/b004576o
_journal_year                    2001
_chemical_formula_sum            'C58 H66 Cu2 N4 O14 P6'
_chemical_formula_weight         1356.05
_chemical_name_systematic
;
 bis(nitrilo-tris(methylenephenylphosphinate)copper(II)Pyridine),
 bis-acetone
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                63.75(4)
_cell_angle_beta                 85.75(4)
_cell_angle_gamma                65.04(4)
_cell_formula_units_Z            1
_cell_length_a                   11.162(5)
_cell_length_b                   12.414(9)
_cell_length_c                   13.967(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1558.5(17)
_computing_molecular_graphics    'ORTEP (Johnson, 1976; Zsolnai, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'enraf nonius cad4'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2385
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2905
_diffrn_reflns_theta_max         19.98
_diffrn_reflns_theta_min         2.78
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.902
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.963
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.2027
_refine_ls_R_factor_obs          0.0686
_refine_ls_shift/esd_max         .634
_refine_ls_shift/esd_mean        0.219
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1899
_refine_ls_wR_factor_obs         0.1435
_reflns_number_observed          1425
_reflns_number_total             2905
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004576o.txt
_cod_data_source_block           Copperdimer
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+0.0000P] 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^)+(0.0878P)^2^+0.0000P] 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        1558.5(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702438