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_4312764
_publ_section_title
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 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 H65 N10 O2 Zn2 3+, 3(Cl O4 -), 2(C2 H3 N)'
_chemical_formula_sum            'C42 H71 Cl3 N12 O14 Zn2'
_chemical_formula_weight         1205.20
_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                 100.734(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.433(2)
_cell_length_b                   13.414(2)
_cell_length_c                   15.575(2)
_cell_measurement_reflns_used    4506
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      2.38
_cell_volume                     2552.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_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      120(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     0.6900
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36706
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  1.058
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.88
_refine_diff_density_rms         0.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4425
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0787P)^2^+4.3138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.158
_refine_ls_wR_factor_ref         0.170
_reflns_number_gt                3437
_reflns_number_total             4425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0345065si20030513_022438_3.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'__atom_sites_solution_primary' tag replaced with
'_atom_sites_solution_primary'.

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

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_sg_symbol_H-M      'P 21/n'
_cod_database_code               4312764