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_7012496
_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            'C24 H36 Cu N6 O6'
_chemical_formula_weight         568.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.436(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9521(19)
_cell_length_b                   11.851(2)
_cell_length_c                   10.868(2)
_cell_measurement_reflns_used    855
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.115
_cell_measurement_theta_min      3.127
_cell_volume                     1271.0(4)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP'
_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      294(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11469
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0.000
_diffrn_standards_number         108
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Gaussian and SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0481P)^2^+0.4730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                2523
_reflns_number_total             3008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211394e.txt
_cod_data_source_block           lfl19
_cod_original_cell_volume        1271.1(4)
_cod_original_sg_symbol_H-M      'P 21/c     '
_cod_database_code               7012496