Observation of a reversible isomorphous phase transition and an interplay of 'sigma-holes' and 'pi-holes' in Fmoc-Leu-psi[CH2-NCS]
Rumpa Pal; Govindappa Nagendra; M. Samarasimhareddy; Vommina V. Sureshbabu; Tayur N. Guru Row; Chem.Commun. 51 (2015) 933–; doi:10.1039/C4cc08751H

data_7116326
_publ_section_title
;
 Observation of a reversible isomorphous phase transition and an interplay
 of 'sigma-holes' and 'pi-holes' in Fmoc-Leu-psi[CH2-NCS]
;
_journal_name_full               Chem.Commun.
_journal_page_first              933
_journal_paper_doi               10.1039/C4cc08751H
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C22 H24 N2 O2 S'
_chemical_formula_sum            'C22 H24 N2 O2 S'
_chemical_formula_weight         380.50
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      76
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2014-11-01 deposited with the CCDC.
2014-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4665(1)
_cell_length_b                   17.4665(1)
_cell_length_c                   13.1291(1)
_cell_measurement_reflns_used    42280
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.1
_cell_measurement_theta_min      2.6
_cell_volume                     4005.41(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_max 0.9998
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       'f\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0851
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            530944
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         50.5794
_diffrn_reflns_theta_min         2.6076
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  1.843
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   gaussian
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.5992
_exptl_crystal_size_mid          0.3100
_exptl_crystal_size_min          0.2556
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_method     ' none'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         42280
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0262P)^2^] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                32688
_reflns_number_total             42280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08751h2.cif
_cod_data_source_block           redo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value ' mixed' changed to 'mixed'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_database_code               7116326