Synthesis of the terpyridyl pendant-arm azamacrocycle 4'-( p-1,4,7-triazacyclonon-1-ylmethylphenyl)-2,2'∶6',2″-terpyridine (L) and complexes of L with copper(II) and nickel(II). Crystal structure of [Cu(HL)(H2O)2][PF6]3
Turonek, Mary L.; Moore, Peter; Errington, William; Journal of the Chemical Society, Dalton Transactions  (2000) 441–; doi:10.1039/a907717k

data_7008974
_publ_section_title
;
 Synthesis of the terpyridyl pendant-arm azamacrocycle
 4'-(&#x200A;p-1,4,7-triazacyclonon-1-ylmethylphenyl)-2,2'&#x2236;6',2&#x2033;-terpyridine
 (L) and complexes of L with copper(II) and nickel(II). Crystal
 structure of [Cu(HL)(H2O)2][PF6]3
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              441
_journal_paper_doi               10.1039/a907717k
_journal_year                    2000
_chemical_formula_sum            'C28 H43 Cu F18 N6 O6 P3'
_chemical_formula_weight         1058.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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-97
_cell_angle_alpha                74.93(3)
_cell_angle_beta                 79.94(3)
_cell_angle_gamma                86.42(3)
_cell_formula_units_Z            2
_cell_length_a                   8.654(2)
_cell_length_b                   11.277(2)
_cell_length_c                   21.593(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.98
_cell_volume                     2003.2(8)
_computing_cell_refinement       MADNES
_computing_data_collection       'MADNES (Plugrath, 1992)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.816
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_device_type
' Delft Instruments FAST TV area-detector diffractometer''
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_sigmaI/netI    0.4276
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9155
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.799
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.545
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         5832
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.544
_refine_ls_R_factor_all          0.1749
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                1706
_reflns_number_total             5832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907717k.txt
_cod_data_source_block           cutp9
_cod_original_cell_volume        2003.2(7)
_cod_database_code               7008974