Dismantling the salen framework: design of new asymmetric silylcyanation catalysts
Ternel, Jérémy; Roussel, Pascal; Agbossou-Niedercorn, Francine; Gauvin, Régis M.; Catal. Sci. Technol. 3 (2013) 580–; doi:10.1039/C2CY20818K

data_1556343
_publ_section_title
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 Dismantling the salen framework: design of new asymmetric silylcyanation
 catalysts
;
_journal_issue                   3
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              580
_journal_paper_doi               10.1039/C2CY20818K
_journal_volume                  3
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C56 H78 Al Cl N4 O6 S2, 4(C6 H6)'
_chemical_formula_sum            'C80 H102 Al Cl N4 O6 S2'
_chemical_formula_weight         1342.28
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6143(3)
_cell_length_b                   13.6143(3)
_cell_length_c                   38.6616(8)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     7165.9(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            76565
_diffrn_reflns_theta_full        28.273
_diffrn_reflns_theta_max         28.273
_diffrn_reflns_theta_min         1.586
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.42
_refine_ls_abs_structure_details 'Flack (1983), 3766 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.09(14)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         4383
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.0010284
_refine_ls_shift/su_mean         0.0000595
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.560 0.661 0.224
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1720
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0751
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              51
_reflns_limit_l_min              0
_reflns_number_gt                5918
_reflns_number_total             8870
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0713
_oxford_refine_ls_scale          0.06366(18)
_oxford_reflns_number_all        8839
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c2cy20818k.txt
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 41 21 2 '
_cod_original_formula_sum        'C80 H102 Al1 Cl1 N4 O6 S2'
_cod_database_code               1556343
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT ENANTIO
RIDE C ( 1,X'S) H ( 2,X'S)
RIDE C ( 2,X'S) H ( 3,X'S)
RIDE C ( 3,X'S) H ( 4,X'S)
RIDE N ( 2,X'S) H ( 5,X'S)
RIDE C ( 4,X'S) H ( 6,X'S) H ( 7,X'S) H ( 8,X'S)
RIDE C ( 7,X'S) H ( 9,X'S) H ( 10,X'S)
RIDE C ( 8,X'S) H ( 11,X'S) H ( 12,X'S)
RIDE C ( 9,X'S) H ( 13,X'S) H ( 14,X'S) H ( 15,X'S)
RIDE C ( 10,X'S) H ( 16,X'S) H ( 17,X'S)
RIDE C ( 13,X'S) H ( 18,X'S)
RIDE C ( 14,X'S) H ( 19,X'S)
RIDE C ( 16,X'S) H ( 20,X'S) H ( 21,X'S)
RIDE C ( 18,X'S) H ( 22,X'S) H ( 23,X'S) H ( 24,X'S)
RIDE C ( 19,X'S) H ( 25,X'S)
RIDE C ( 20,X'S) H ( 26,X'S)
RIDE C ( 21,X'S) H ( 27,X'S)
RIDE C ( 24,X'S) H ( 28,X'S)
RIDE C ( 25,X'S) H ( 29,X'S) H ( 30,X'S) H ( 31,X'S)
RIDE C ( 26,X'S) H ( 32,X'S)
RIDE C ( 27,X'S) H ( 33,X'S)
RIDE C ( 28,X'S) H ( 52,X'S)
RIDE C ( 29,X'S) H ( 34,X'S)
RIDE C ( 30,X'S) H ( 35,X'S)
RIDE C ( 31,X'S) H ( 36,X'S)
RIDE C ( 32,X'S) H ( 37,X'S)
RIDE C ( 33,X'S) H ( 38,X'S)
RIDE C ( 34,X'S) H ( 53,X'S)
RIDE C ( 35,X'S) H ( 39,X'S)
RIDE C ( 36,X'S) H ( 40,X'S) H ( 41,X'S) H ( 42,X'S)
RIDE C ( 37,X'S) H ( 43,X'S)
RIDE C ( 38,X'S) H ( 44,X'S)
RIDE C ( 39,X'S) H ( 45,X'S)
RIDE C ( 40,X'S) H ( 46,X'S) H ( 47,X'S) H ( 48,X'S)
RIDE C ( 41,X'S) H ( 49,X'S) H ( 50,X'S) H ( 51,X'S)
END
;
_iucr_refine_instruction_details_restraints
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NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
DISTANCE 1.400000 , 0.010000 = C(26) TO C(30)
DISTANCE 1.400000 , 0.010000 = C(24) TO C(28)
DISTANCE 1.400000 , 0.010000 = C(24) TO C(27)
DISTANCE 1.400000 , 0.010000 = C(27) TO C(32)
DISTANCE 1.400000 , 0.010000 = C(32) TO C(33)
DISTANCE 1.400000 , 0.010000 = C(33) TO C(34)
DISTANCE 1.400000 , 0.010000 = C(28) TO C(34)
DISTANCE 1.400000 , 0.010000 = C(31) TO C(37)
DISTANCE 1.400000 , 0.005000 = C(30) TO C(31)
DISTANCE 1.400000 , 0.010000 = C(26) TO C(30)
DISTANCE 1.400000 , 0.005000 = C(35) TO C(39)
DISTANCE 1.400000 , 0.010000 = C(35) TO C(38)
DISTANCE 1.400000 , 0.010000 = C(38,8,1,0,0,-1) TO C(39)
DISTANCE 1.540000 , 0.002000 = C(23) TO C(40)
END
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