A Lewis acid-mediated conformational switch.
Knipe, Peter C.; Lingard, Hannah; Jones, Ian M.; Thompson, Sam; Hamilton, Andrew D.; Organic & biomolecular chemistry 12 (2014) 7937–7941; doi:10.1039/c4ob01556h

data_7154010
_publ_section_title
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 A Lewis acid-mediated conformational switch.
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_journal_issue                   40
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7937
_journal_page_last               7941
_journal_paper_doi               10.1039/c4ob01556h
_journal_volume                  12
_journal_year                    2014
_chemical_compound_source        syn
_chemical_formula_moiety         'C30 H22 Cl3 N3 O4'
_chemical_formula_sum            'C30 H22 Cl3 N3 O4'
_chemical_formula_weight         594.88
_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   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                94.2169(9)
_cell_angle_beta                 90.9044(9)
_cell_angle_gamma                109.4296(11)
_cell_formula_units_Z            2
_cell_length_a                   9.3185(2)
_cell_length_b                   11.8470(2)
_cell_length_c                   13.2263(3)
_cell_measurement_reflns_used    6124
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1372.00(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29697
_diffrn_reflns_theta_full        26.976
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         5.130
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612.000
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0492
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6242
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.0020352
_refine_ls_shift/su_mean         0.0000301
_refine_ls_structure_factor_coef Fsqd
_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: 
 28.8 38.6 12.0 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1303
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1303
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4950
_reflns_number_total             6242
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.13
_oxford_diffrn_Wilson_scale      0.69
_oxford_refine_ls_r_factor_ref   0.0840
_oxford_refine_ls_scale          1.170(4)
_oxford_reflns_number_all        6242
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE N   (   7,X'S) H   (  71,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE N   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 363,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
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SAME  C(37)  CL(38)  CL(39)  CL(40)  AND 
CONT  C(37)  CL(39)  CL(40)  CL(38)  AND 
CONT  C(37)  CL(40)  CL(38)  CL(39)  AND 
CONT  C(37)  CL(138)  CL(139)  CL(140)  AND 
CONT  C(37)  CL(139)  CL(140)  CL(138)  AND 
CONT  C(37)  CL(140)  CL(138)  CL(139) 
SIMU  0.01   C(37)  CL(38)  CL(39)  CL(40)  AND 
CONT  C(37)  CL(39)  CL(40)  CL(38)  AND 
CONT  C(37)  CL(40)  CL(38)  CL(39)  AND 
CONT  C(37)  CL(138)  CL(139)  CL(140)  AND 
CONT  C(37)  CL(139)  CL(140)  CL(138)  AND 
CONT  C(37)  CL(140)  CL(138)  CL(139) 
DELU  0.01   C(37)  CL(38)  CL(39)  CL(40)  AND 
CONT  C(37)  CL(39)  CL(40)  CL(38)  AND 
CONT  C(37)  CL(40)  CL(38)  CL(39)  AND 
CONT  C(37)  CL(138)  CL(139)  CL(140)  AND 
CONT  C(37)  CL(139)  CL(140)  CL(138)  AND 
CONT  C(37)  CL(140)  CL(138)  CL(139) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            c4ob01556h2.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 

 Adding full bibliography for 7154010.cif.
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_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7154010