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_7113075
_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 Nd O8, C3 H7 N O'
_chemical_formula_sum            'C39 H40 N5 Nd O9'
_chemical_formula_weight         867.00
_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                91.021(5)
_cell_angle_beta                 102.172(5)
_cell_angle_gamma                95.652(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8275(6)
_cell_length_b                   10.7284(7)
_cell_length_c                   19.2871(12)
_cell_measurement_reflns_used    18254
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.385
_cell_measurement_theta_min      1.905
_cell_volume                     1976.6(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'image plate (34 cm diameter / schwenk)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details      ' 158 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0438
_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       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11341
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_T_max  0.8750
_exptl_absorpt_correction_T_min  0.7709
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'HABITUS (Herrendorf et al., 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         6505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                5765
_reflns_number_total             6505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc00949k.txt
_cod_data_source_block           ip2-558
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               7113075