Synthesis, structure and reactions of the most twisted amide
Kirby, Anthony J.; Komarov, Igor V.; Feeder, Neil; Journal of the Chemical Society, Perkin Transactions 2  (2001) 522–; doi:10.1039/b008270h

data_7216925
_publ_section_title
;
 Synthesis, structure and reactions of the most twisted amide
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              522
_journal_paper_doi               10.1039/b008270h
_journal_year                    2001
_chemical_formula_sum            'C14 H26 I N O'
_chemical_formula_weight         351.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.76(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.130(11)
_cell_length_b                   8.810(7)
_cell_length_c                   14.747(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      30
_cell_volume                     1543(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Rigaku R-Axis IIc'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
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_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10426
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    2.064
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.312
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2606
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.312
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_obs          0.0872
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+7.9419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1572
_refine_ls_wR_factor_obs         0.1473
_reflns_number_observed          2385
_reflns_number_total             2615
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b008270h.txt
_cod_data_source_block           ak9705
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+7.9419P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+7.9419P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1542.9(22)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7216925