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_7224517
_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         '2(C30 H28 N6 Ni1 S2), (C14 H10), (C6 H6)'
_chemical_formula_sum            'C80 H72 N12 Ni2 S4'
_chemical_formula_weight         1447.32
_chemical_name_systematic
'Tetrakisvinylpyridine bisisothiocyanato nickel(II) phenanthrene.benzene'
_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                100.059(2)
_cell_angle_beta                 100.131(2)
_cell_angle_gamma                102.908(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4819(9)
_cell_length_b                   16.8458(14)
_cell_length_c                   22.5690(19)
_cell_measurement_reflns_used    89108
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.23
_cell_volume                     3727.6(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 0.994
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            89108
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.613
_diffrn_reflns_theta_min         1.272
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Triclinic
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         17210
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0576P)^2^+2.0225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12869
_reflns_number_total             17210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02185e2.cif
_cod_data_source_block           D_H3_PheBen
_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               7224517
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.740
_shelx_estimated_absorpt_t_max   0.814
_shelx_res_checksum              63299