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_7113074
_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         'C38 H40 N Nd O10'
_chemical_formula_sum            'C38 H40 N Nd O10'
_chemical_formula_weight         814.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.944(3)
_cell_length_b                   17.819(4)
_cell_length_c                   12.906(3)
_cell_measurement_reflns_used    10488
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      1.72
_cell_volume                     3661.6(14)
_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 0.817
_diffrn_measured_fraction_theta_max 0.817
_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  0.1028
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14041
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.72
_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    1.475
_exptl_absorpt_correction_T_max  0.9299
_exptl_absorpt_correction_T_min  0.8665
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED32 (Stoe & Cie GmbH)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.592
_refine_diff_density_min         -2.750
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7961
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0759
_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^)+(0.1064P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1979
_reflns_number_gt                4535
_reflns_number_total             7961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc00949k.txt
_cod_data_source_block           p21c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        3661.6(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7113074