Unsymmetrically substituted side-bridged cyclam derivatives and their Cu(ii) and Zn(ii) complexes
Plutnar, Jan; Havlíčková, Jana; Kotek, Jan; Hermann, Petr; Lukeš, Ivan; New Journal of Chemistry 32 (2008) 496–; doi:10.1039/b709747f

data_7051776
_publ_section_title
;
 Unsymmetrically substituted side-bridged cyclam derivatives and their
 Cu(ii) and Zn(ii) complexes
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              496
_journal_paper_doi               10.1039/b709747f
_journal_volume                  32
_journal_year                    2008
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C19 H31 Br Cu N5 O2, F6 P'
_chemical_formula_sum            'C19 H31 Br Cu F6 N5 O2 P'
_chemical_formula_weight         649.91
_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                73.592(3)
_cell_angle_beta                 84.539(5)
_cell_angle_gamma                80.636(4)
_cell_formula_units_Z            2
_cell_length_a                   6.9960(4)
_cell_length_b                   10.2570(8)
_cell_length_c                   17.8780(15)
_cell_measurement_reflns_used    9051
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.00
_cell_volume                     1212.60(16)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9051
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.688
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.544
_refine_diff_density_min         -1.984
_refine_diff_density_rms         0.452
_refine_ls_extinction_coef       0.32(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.973
_refine_ls_R_factor_all          0.2134
_refine_ls_R_factor_gt           0.1759
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4889
_refine_ls_wR_factor_ref         0.5043
_reflns_number_gt                3452
_reflns_number_total             5090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b709747f.txt
_cod_data_source_block           pled
_cod_database_code               7051776