Monitoring the stepwise assembly of a 3-D framework from a supramolecular lanthanoid synthon by in situ infrared spectroscopy.
Andrews, Philip C.; Gee, William J.; Junk, Peter C.; Krautscheid, Harald; MacLellan, Jonathan G.; Chemical communications (Cambridge, England) 46 (2010) 5948–5950; doi:10.1039/c0cc00949k

data_7113076
_publ_section_title
;
 Monitoring the stepwise assembly of a 3-D framework from a supramolecular
 lanthanoid synthon by in situ infrared spectroscopy.
;
_journal_issue                   32
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5948
_journal_page_last               5950
_journal_paper_doi               10.1039/c0cc00949k
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C36 H33 N4 O8 Tb, C3 H7 N O'
_chemical_formula_sum            'C39 H40 N5 O9 Tb'
_chemical_formula_weight         881.68
_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                91.16(3)
_cell_angle_beta                 101.99(3)
_cell_angle_gamma                95.68(3)
_cell_formula_units_Z            2
_cell_length_a                   9.774(2)
_cell_length_b                   10.682(2)
_cell_length_c                   19.281(4)
_cell_measurement_reflns_used    19623
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.85
_cell_measurement_theta_min      2.16
_cell_volume                     1957.7(7)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Australian synchrotron MX2'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77487
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19623
_diffrn_reflns_theta_full        23.85
_diffrn_reflns_theta_max         23.85
_diffrn_reflns_theta_min         2.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.866
_exptl_absorpt_correction_T_max  0.9636
_exptl_absorpt_correction_T_min  0.9461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.690
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         5250
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+3.9763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                5226
_reflns_number_total             5250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc00949k.txt
_cod_data_source_block           wg4
_cod_database_code               7113076