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_4312763
_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_absolute_configuration ad
_chemical_formula_moiety
'C38 H64 Cu2 N10 O2 2+, 2(B F4 -), 0.5(C2 H3 N)'
_chemical_formula_sum            'C39 H65.5 B2 Cu2 F8 N10.5 O2'
_chemical_formula_weight         1014.22
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   28.064(3)
_cell_length_b                   48.112(5)
_cell_length_c                   15.996(2)
_cell_measurement_reflns_used    7119
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.1
_cell_measurement_theta_min      2.15
_cell_volume                     21598(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL'
_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_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6861
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_sigmaI/netI    0.065
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10688
_diffrn_reflns_theta_full        19.15
_diffrn_reflns_theta_max         19.15
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8464
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         3964
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0766
_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^)+(0.1606P)^2^+43.7001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.202
_refine_ls_wR_factor_ref         0.218
_reflns_number_gt                3295
_reflns_number_total             3964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0345065si20030513_022438_2.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:
'__computing_data_collection' tag replaced with
'_computing_data_collection'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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_original_formula_sum        C39H65.5B2Cu2F8N10.5O2
_cod_database_code               4312763