Cyclam Functionalization through Isocyanate Insertion in Zr-N Bonds
Luis G. Alves; Ana M. Martins; Inorganic Chemistry 51 (2012) 10–12; doi:10.1021/ic201750y

data_4327808
_publ_contact_author_address
;Centro de Qu\'imica Estrutural
Instituto Superior T\'ecnico
Av. Rovisco Pais 1
1049-001 Lisboa
Portugal
;
_publ_contact_author_email       ana.martins@ist.utl.pt
_publ_contact_author_name        'Ana M. Martins'
_publ_contact_author_phone       '+351 218419172'
_publ_section_title
;
 Cyclam Functionalization through Isocyanate Insertion in Zr-N Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10
_journal_page_last               12
_journal_paper_doi               10.1021/ic201750y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C30 H48 N4 O2 Zr'
_chemical_formula_sum            'C30 H48 N4 O2 Zr'
_chemical_formula_weight         587.94
_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                95.37(3)
_cell_angle_beta                 99.61(2)
_cell_angle_gamma                108.22(2)
_cell_formula_units_Z            2
_cell_length_a                   8.895(4)
_cell_length_b                   9.066(4)
_cell_length_c                   19.779(8)
_cell_measurement_reflns_used    672
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.90
_cell_volume                     1475.6(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1099
_diffrn_reflns_av_sigmaI/netI    0.1768
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12017
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.9606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0106P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                3157
_reflns_number_total             5386
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201750y_si_001_2.cif
_cod_data_source_block           2a
_cod_database_code               4327808