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_7224515
_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         '4(C30 H28 N6 Ni1 S2), 3(C13 H10)'
_chemical_formula_sum            'C159 H142 N24 Ni4 S8'
_chemical_formula_weight         2880.61
_chemical_name_systematic
'Tetrakisvinylpyridine bisisothiocyanato nickel(II) fluorene'
_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
_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                84.603(2)
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_cell_angle_gamma                74.788(3)
_cell_formula_units_Z            1
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_cell_measurement_reflns_used    94121
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.390
_cell_measurement_theta_min      2.866
_cell_volume                     3690.4(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1\% \f scans and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_unetI/netI     0.0919
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            94121
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         2.866
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.675
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_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1504
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_refine_diff_density_max         0.538
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     986
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_refine_ls_number_restraints     245
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0468P)^2^+0.3492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7658
_reflns_number_total             14995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02185e2.cif
_cod_data_source_block           H3Flu_I_Plate
_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_original_cell_volume        3690.3(5)
_cod_database_code               7224515
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.860
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              33184