Crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-<i>{κ</i>}^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')(1,6,7,12-tetraazaperylene-<i>{κ</i>}^2^<i>N</i>^1^,<i>N</i>^12^)ruthenium(II) bis(hexafluoridophosphate) acetonitrile 1.422-solvate
Brietzke, Thomas; Rottke, Falko Otto; Kelling, Alexandra; Schilde, Uwe; Holdt, Hans-Jürgen; Acta Crystallographica Section E 70 (2014) 265–268; doi:10.1107/S1600536814021060

data_2240050
_publ_section_title
;
 Crystal structure of
 (2,11-diaza[3.3](2,6)pyridinophane-<i>{\k</i>}^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')(1,6,7,12-tetraazaperylene-<i>{\k</i>}^2^<i>N</i>^1^,<i>N</i>^12^)ruthenium(II)
 bis(hexafluoridophosphate) acetonitrile 1.422-solvate
;
_journal_coeditor_code           ZL2602
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              265
_journal_page_last               268
_journal_paper_doi               10.1107/S1600536814021060
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Ru (C14 H16 N4) (C16 H8 N4)] (P F6)2 , 1.422C2 H3 N'
_chemical_formula_moiety         'C30 H24 N8 Ru, 2(P F6), 1.422(C2 H3 N)'
_chemical_formula_sum            'C32.84 H28.27 F12 N9.42 P2 Ru'
_chemical_formula_weight         946.11
_chemical_name_systematic
;
(2,11-Diaza[3.3](2,6)pyridinophane-\
\k^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')(1,6,7,12-tetraazaperylene-\
\k^2^<i>N</i>^1^,<i>N</i>^12^)ruthenium(II) bis(hexafluoridophosphate) 
acetonitrile 1.422-solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 97.938(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7027(3)
_cell_length_b                   21.7157(7)
_cell_length_c                   13.9377(4)
_cell_measurement_reflns_used    63561
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      1.47
_cell_volume                     3508.08(18)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2011)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2011)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2011)
;
_computing_molecular_graphics
;
MERCURY (Macrae <i>et al.</i>,  2006),
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2008),
<i>SHELXLE</i> (H\"ubschle <i>et al.</i>,  2011),
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60767
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.314
_diffrn_reflns_theta_min         1.748
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.8428
_exptl_absorpt_correction_T_min  0.6129
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED; Stoe & Cie, 2011)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       prism
_exptl_crystal_F_000             1893.4
_exptl_crystal_size_max          1.300
_exptl_crystal_size_mid          0.650
_exptl_crystal_size_min          0.310
_refine_diff_density_max         1.837
_refine_diff_density_min         -1.216
_refine_ls_extinction_coef       0.0041(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         9454
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+2.1270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1461
_reflns_number_gt                7744
_reflns_number_total             9454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2602sup1.cf
_cod_data_source_block           I
_cod_database_code               2240050
_cod_database_fobs_code          2240050
_shelx_hkl_checksum              93265
_shelx_res_checksum              51898
_shelxl_version_number           201.4