Werner clathrate formation with polyaromatic hydrocarbons: comparison of different crystallisation methods
Wicht, Merrill M.; Su, Hong; Báthori, Nikoletta B.; Nassimbeni, Luigi R.; CrystEngComm 18 (2016) 2509–; doi:10.1039/C5CE02185E

data_7224518
_publ_section_title
;
 Werner clathrate formation with polyaromatic hydrocarbons: comparison of
 different crystallisation methods
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2509
_journal_paper_doi               10.1039/C5CE02185E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C30 H28 N6 Ni1 S2, 0.625(C14 H10)'
_chemical_formula_sum            'C38.75 H34.25 N6 Ni S2'
_chemical_formula_weight         706.80
_chemical_name_systematic
'Tetrakisvinylpyridine bisisothiocycanato nickel(II) phenanthrene'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-06 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                81.874(2)
_cell_angle_beta                 83.128(2)
_cell_angle_gamma                76.0070(10)
_cell_formula_units_Z            4
_cell_length_a                   10.3117(8)
_cell_length_b                   16.8992(14)
_cell_length_c                   22.3886(17)
_cell_measurement_reflns_used    39815
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.094
_cell_measurement_theta_min      2.043
_cell_volume                     3732.8(5)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker 2004)'
_computing_molecular_graphics    'X-seed (Barbour, 1999)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Kappa Duo Apex II diffractometer'
_diffrn_measurement_method       '1.2\% \f scans and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39815
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.094
_diffrn_reflns_theta_min         2.043
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             1475
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         16209
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0955P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8644
_reflns_number_total             16209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02185e2.cif
_cod_data_source_block           H3Phe
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7224512--7224520.cif.
;
_cod_database_code               7224518
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              25688