Hexane-1,6-diammonium dichloride at 100 K Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2
Thierry Maris; Personal communication to COD  (2023) –; doi:

data_3500134
_publ_section_references
;

Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H.
 (2015). Acta Cryst. A71, 59-75.

Bruker      (2021). <i>APEX4</i>. Bruker AXS Inc., Madison,
Wisconsin, USA

Bruker      (2020). <i>SAINT</i>. Bruker AXS Inc., Madison,
Wisconsin, USA

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Kleemiss, F., Dolomanov, O.V., Bodensteiner, M., Peyerimhoff, N., Midgley, M.,
Bourhis, L.J., Genoni, A., Malaspina, L.A., Jayatilaka, D., Spencer, J.L.,
White, F., Grundkoetter-Stock, B, Steinhauer, S., Lentz, D., Puschmann, H.,
Grabowsky, S. (2021), Chem. Sci., 12, 1675-1692.

Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). <i>J. Appl.
Cryst.</i> <b>48</b>, 3--10.

Sheldrick, G. M. (2015). <i>Acta Cryst.</i> A<b>71</b>, 3--8.

;
_publ_section_title
;
 Hexane-1,6-diammonium dichloride at 100 K Refinement using NoSpherA2, an
 implementation of NOn-SPHERical Atom-form-factors in Olex2
;
_journal_name_full               'Personal communication to COD'
_journal_year                    2023
_chemical_formula_moiety         'C6 H18 N2, 2(Cl)'
_chemical_formula_sum            'C6 H18 Cl2 N2'
_chemical_formula_weight         189.128
_chemical_name_common            'Hexane-1,6-diammonium dichloride'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2022-07-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.534(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.5560(3)
_cell_length_b                   14.1107(9)
_cell_length_c                   15.5164(10)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100
_cell_measurement_theta_max      78.882
_cell_measurement_theta_min      2.478
_cell_volume                     997.48(11)
_computing_cell_refinement
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Bruker CMOS Photon III '
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9921
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9921
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30652
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9921
_diffrn_reflns_theta_full        53.5942
_diffrn_reflns_theta_max         79.06
_diffrn_reflns_theta_min         3.68
_diffrn_source                   'Metal Jet'
_diffrn_source_current           2.86
_diffrn_source_power             0.199370
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_source_voltage           69.71
_exptl_absorpt_coefficient_mu    3.568
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.6289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1331 before and 0.0797 after correction.
The Ratio of minimum to maximum transmission is 0.8339.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       Block
_exptl_crystal_F_000             411.215
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_special_details
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker Venture diffractometer equipped with a Photon III CMOS Detector,
a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance 
was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode.
;
_refine_diff_density_max         0.3507
_refine_diff_density_min         -0.3613
_refine_diff_density_rms         0.0582
_refine_ls_d_res_high            0.6831
_refine_ls_d_res_low             10.4392
_refine_ls_goodness_of_fit_ref   1.0623
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0623
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+0.1802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0556
_refine_special_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by 
employing cluster charges or modelled using implicit solvation models, 
depending on the software used.
The following options were used:
   SOFTWARE:       ORCA
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   High
   METHOD:         PBE
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2022-07-28_14-06-48
;
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3218
_reflns_number_total             3267
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6cl100k.cif
_cod_data_source_block           c6cl100k
_cod_database_code               3500134
_cod_database_fobs_code 3500134