N-Monofunctionalized 1,4,7-Triazacyclononane Macrocycles as Building Blocks in Inorganic Crystal Engineering
Patrick C. McGowan; Thomas J. Podesta; Mark Thornton-Pett; Inorganic Chemistry 40 (2001) 1445–1453; doi:10.1021/ic0006854

data_4319431
_publ_contact_author
;
   Patrick McGowan
   School of Chemistry 
   University of Leeds
   Leeds LS2 9JT
   UK
;
_publ_contact_author_email       patrickm@chem.leeds.ac.uk
_publ_contact_author_fax         '+44 (0)113 2336565'
_publ_contact_author_phone       '+44 (0)113 2336404'
_publ_section_title
;
 N-Monofunctionalized 1,4,7-Triazacyclononane Macrocycles as Building
 Blocks in Inorganic Crystal Engineering
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1445
_journal_page_last               1453
_journal_paper_doi               10.1021/ic0006854
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C12 H26 Mo N4 O6'
_chemical_formula_weight         418.31
_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                72.3960(18)
_cell_angle_beta                 82.723(2)
_cell_angle_gamma                89.190(2)
_cell_formula_units_Z            4
_cell_length_a                   7.0029(2)
_cell_length_b                   14.9415(6)
_cell_length_c                   17.2168(4)
_cell_measurement_temperature    150(2)
_cell_volume                     1702.71(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets 
   1 degree phi exposures for chi=0 degree settings
   1 degree omega exposures for chi=90 degree settings
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20790
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.9495
_exptl_absorpt_correction_T_min  0.7442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
 See R.H. Blessing, Acta Cryst (1995), A51, 33-38   
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.220
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0041(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         7497
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+1.1450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                6334
_reflns_number_total             7497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0006854_1.cif
_cod_data_source_block           tjp5
_cod_database_code               4319431