Synthesis and characterisation of pendant-arm amino derivatives of 1,4,7-triazacyclononane and alkyl-bridged bis(1,4,7-triazacyclononane) macrocycles and complexation to Cu(II)
Blake, Alexander J.; Danks, Jonathan P.; Li, Wan-Sheung; Lippolis, Vito; Schröder, Martin; Journal of the Chemical Society, Dalton Transactions  (2000) 3034–; doi:10.1039/b002626n

data_7009670
_publ_section_title
;
 Synthesis and characterisation of pendant-arm amino derivatives of
 1,4,7-triazacyclononane and alkyl-bridged bis(1,4,7-triazacyclononane)
 macrocycles and complexation to Cu(II)
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3034
_journal_paper_doi               10.1039/b002626n
_journal_year                    2000
_chemical_formula_sum            'C19 H39 Cu F12 N8 P2'
_chemical_formula_weight         733.06
_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                107.220(10)
_cell_angle_beta                 90.88(2)
_cell_angle_gamma                118.530(10)
_cell_formula_units_Z            2
_cell_length_a                   11.786(2)
_cell_length_b                   12.189(2)
_cell_length_c                   12.849(2)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      12.5
_cell_volume                     1521.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       omega/theta
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5904
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  0.5417
_exptl_absorpt_correction_T_min  0.493
_exptl_absorpt_correction_type   psi/scans
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    riding/model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         5364
_refine_ls_number_restraints     1056
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+2.1289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                4738
_reflns_number_total             5364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002626n.txt
_cod_data_source_block           dicuam
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+2.1289P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+2.1289P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1521.8(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009670