Coordination Chemistry of a New Cofacial Binucleating Macropolycycle Derived from 1,4,7-Triazacyclononane
Lorenzo Tei; Massimiliano Arca; M. Carla Aragoni; Andrea Bencini; Alexander J. Blake; Claudia Caltagirone; Francesco A. Devillanova; Patrizia Fornasari; Alessandra Garau; Francesco Isaia; Vito Lippolis; Martin Schröder; Simon J. Teat; Barbara Valtancoli; Inorganic Chemistry 42 (2003) 8690–8701; doi:10.1021/ic0345065

data_4312762
_publ_section_title
;
 Coordination Chemistry of a New Cofacial Binucleating Macropolycycle
 Derived from 1,4,7-Triazacyclononane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8690
_journal_page_last               8701
_journal_paper_doi               10.1021/ic0345065
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C38 H72 N10 O2 6+, 6(Cl O4 -), 8(H2 O)'
_chemical_formula_sum            'C38 H88 Cl6 N10 O34'
_chemical_formula_weight         1441.88
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.796(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.457(2)
_cell_length_b                   8.282(2)
_cell_length_c                   29.319(5)
_cell_measurement_reflns_used    1234
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.01
_cell_measurement_theta_min      2.85
_cell_volume                     3186.5(11)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       omega
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.132
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6237
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sphenoid
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6237
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.1760
_refine_ls_R_factor_gt           0.0796
_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^)+(0.1117P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1999
_refine_ls_wR_factor_ref         0.2320
_reflns_number_gt                2259
_reflns_number_total             6237
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0345065si20030513_022438_1.cif
_cod_data_source_block           gdcage
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'placed geometrically' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4312762