O-Benzylated-calix[4]arenes as ancillary ligands in organolanthanide chemistry
Estler, Frank; Herdtweck, Eberhardt; Anwander, Reiner; Journal of the Chemical Society, Dalton Transactions  (2002) 3088–; doi:10.1039/b205200h

data_7011869
_publ_section_title
;
 O-Benzylated-calix[4]arenes as ancillary ligands in organolanthanide
 chemistry
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3088
_journal_paper_doi               10.1039/b205200h
_journal_year                    2002
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C62 H80 N O4 Sc Si2, 3(C7 H8)'
_chemical_formula_sum            'C83 H104 N O4 Sc Si2'
_chemical_formula_weight         1280.81
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 92.577(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5600(4)
_cell_length_b                   24.5441(7)
_cell_length_c                   17.2735(4)
_cell_measurement_reflns_used    37074
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      1.66
_cell_volume                     7437.3(3)
_computing_cell_refinement       'DENZO (Nonius, 2000b)'
_computing_data_collection       'Kappa-CCD Control Software (Nonius, 2000a)'
_computing_data_reduction        'DENZO (Nonius, 2000b)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean '18  # 9 for binned mode'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Kappa CCD (Nonius)'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0066
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12313
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.9233
_exptl_absorpt_correction_T_min  0.8934
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
; 
Neither decay correction nor absorption correction necessary
Denzo-SNM; Scale-Pack
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         12306
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+13.9657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                11125
_reflns_number_total             12306
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            b205200h.txt
_cod_data_source_block           ESTB-4090-123
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7011869