Asymmetric synthesis of ethano-Tröger bases using CuTC-catalyzed diazo decomposition reactions.
Sharma, Ankit; Besnard, Céline; Guénée, Laure; Lacour, Jérôme; Organic & biomolecular chemistry 10 (2012) 966–969; doi:10.1039/c1ob06751f

data_7152197
_publ_section_title
;
 Asymmetric synthesis of ethano-Tr\"oger bases using CuTC-catalyzed diazo
 decomposition reactions.
;
_journal_issue                   5
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              966
_journal_page_last               969
_journal_paper_doi               10.1039/c1ob06751f
_journal_volume                  10
_journal_year                    2012
_chemical_formula_moiety         'C22 H24 N2 O3'
_chemical_formula_sum            'C22 H24 N2 O3'
_chemical_formula_weight         364.44
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 93.201(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.051(2)
_cell_length_b                   7.5405(6)
_cell_length_c                   28.226(4)
_cell_measurement_reflns_used    15643
_cell_measurement_temperature    220
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_cell_measurement_theta_min      1
_cell_volume                     3623.4(7)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1996)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      220
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            11824
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_diffrn_reflns_theta_max         25.657
_diffrn_reflns_theta_min         1.445
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
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_exptl_crystal_colour            orange
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
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_refine_diff_density_max         0.34
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_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:
18.2 21.2 6.66
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1015
_refine_ls_wR_factor_gt          0.1011
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_reflns_limit_k_min              0
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_reflns_limit_l_min              0
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_reflns_number_total             3385
_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   0.0721
_oxford_refine_ls_scale          0.4684(7)
_oxford_reflns_number_all        3373
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c1ob06751f.txt
_cod_data_source_block           5c
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3623.3(7)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               7152197