Macrocyclic ligand design. Interaction of a series of successively N-benzylated derivatives of 1,4,8,11-tetraazacyclotetradecane (cyclam) with copper(ii) and nickel(ii)
Dong, Ying; Lawrance, Geoffrey A.; Lindoy, Leonard F.; Turner, Peter; Dalton Transactions  (2003) 1567–; doi:10.1039/b211394e

data_7012497
_publ_section_title
;
 Macrocyclic ligand design. Interaction of a series of successively
 N-benzylated derivatives of 1,4,8,11-tetraazacyclotetradecane (cyclam)
 with copper(ii) and nickel(ii)
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1567
_journal_paper_doi               10.1039/b211394e
_journal_year                    2003
_chemical_formula_sum            'C40 H58 Cu N6 O9'
_chemical_formula_weight         830.46
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.129(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.200(12)
_cell_length_b                   9.471(5)
_cell_length_c                   18.229(9)
_cell_measurement_reflns_used    935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.546
_cell_measurement_theta_min      3.421
_cell_volume                     4113(4)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics    'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21311
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0.15
_diffrn_standards_number         212
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   'numerical and empirical'
_exptl_absorpt_process_details
;
Gaussian (XPREP, Bruker 1995) and SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatc
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4881
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0936P)^2^+3.6807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1420
_reflns_number_gt                4183
_reflns_number_total             4881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211394e.txt
_cod_data_source_block           lfl27
_cod_original_sg_symbol_H-M      'C 2/c      '
_cod_database_code               7012497