Polymorphism and solid-to-solid phase transitions of a simple organic molecule, 3-chloroisonicotinic acid
Long, Sihui; Zhou, Panpan; Parkin, Sean; Li, Tonglei; CrystEngComm 17 (2015) 2389–; doi:10.1039/C4CE02563F

data_7219517
_publ_section_title
;
 Polymorphism and solid-to-solid phase transitions of a simple organic
 molecule, 3-chloroisonicotinic acid
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2389
_journal_paper_doi               10.1039/C4CE02563F
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 H4 Cl N O2'
_chemical_formula_sum            'C6 H4 Cl N O2'
_chemical_formula_weight         157.55
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014/7 and CIFFIX'
_audit_update_record
;
2015-02-02 deposited with the CCDC.
2015-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                61.6975(14)
_cell_angle_beta                 80.0002(12)
_cell_angle_gamma                89.5122(12)
_cell_formula_units_Z            1
_cell_length_a                   3.6779(1)
_cell_length_b                   6.9371(1)
_cell_length_c                   7.0372(2)
_cell_measurement_reflns_used    667
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     155.117(7)
_computing_cell_refinement       '<i>SCALEPACK</i> (Otwinowski & Minor, 2006)'
_computing_data_collection       '<i>COLLECT</i> (Nonius, 1998)'
_computing_data_reduction        '<i>DENZO-SMN</i> (Otwinowski & Minor, 2006)'
_computing_molecular_graphics    '<i>XP in SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELX</i> (Sheldrick, 2008) and <i>CIFFIX</i> (Parkin, 2013)'
_computing_structure_refinement  '<i>SHELXL-2014/7</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans at fixed \c = 55\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_number            1334
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         5.882
_diffrn_source                   'fine-focus sealed-tube'
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.9482
_exptl_absorpt_correction_T_min  0.8137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       block
_exptl_crystal_F_000             80
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
; 
Flack 'x' determined using 651 quotients [(I+)-(I-)]/[(I+)+(I-)] 
[Parsons, Flack and Wagner (2013)]. 
;
_refine_ls_abs_structure_Flack   0.010(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1334
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0164
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0461
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    0.937
_reflns_Friedel_fraction_max     0.921
_reflns_number_gt                1332
_reflns_number_total             1334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce02563f2.cif
_cod_data_source_block           III
_cod_depositor_comments
'Adding full bibliography for 7219515--7219517.cif.'
_cod_database_code               7219517
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.814
_shelx_estimated_absorpt_t_max   0.948
_exptl_absorpt_special_details
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by x-ray beam inhomogeneity, goniometer imperfection, crystal longer than 
the x-ray beam cross section, absorption by the crystal mounting fibre etc. 
These account, by and large, for much of the difference between estimated 
values of Tmin and Tmax and the _exptl_absorpt_correction_ values. 
;
_shelx_res_checksum              7351