Crystal structure of [1,1′′′-bis(pyrimidin-2-yl)-4,4′:2′,2′′:4′′,4′′′-quaterpyridine-1,1′′′-diium-κ2N1′,N1′′]bis[2-(pyridin-2-yl)phenyl-κ2N,C1]iridium(III) tris(hexafluoridophosphate) acetonitrile trisolvate
Coe, Benjamin J.; Peers, Martyn K.; Raftery, James; Scrutton, Nigel S.; Acta Crystallographica Section E Crystallographic Communications 71 (2015) 879–; doi:10.1107/S2056989015012463

data_2020017
_publ_section_title
;
 Crystal structure of
 [1,1&#x2032;&#x2032;&#x2032;-bis(pyrimidin-2-yl)-4,4&#x2032;:2&#x2032;,2&#x2032;&#x2032;:4&#x2032;&#x2032;,4&#x2032;&#x2032;&#x2032;-quaterpyridine-1,1&#x2032;&#x2032;&#x2032;-diium-\k2N1&#x2032;,N1&#x2032;&#x2032;]bis[2-(pyridin-2-yl)phenyl-\k2N,C1]iridium(III)
 tris(hexafluoridophosphate) acetonitrile trisolvate
;
_journal_coeditor_code           ZL2625
_journal_issue                   8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              879
_journal_paper_doi               10.1107/S2056989015012463
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Ir (C11 H8 N)2 (C28 H20 N8)] (P F6)3, 3C2 H3 N'
_chemical_formula_sum            'C56 H45 F18 Ir N13 P3'
_chemical_formula_weight         1527.16
_chemical_name_systematic
;[1,1'''-Bis(pyrimidin-2-yl)-4,4':2',2'':4'',4'''-quaterpyridine-1,1'''-diium-\k^2^<i>N</i>^1'^,<i>N</i>^1''^]bis[2-(pyridin-2-yl)phenyl-\k^2^<i>N</i>,<i>C</i>^1^]iridium(III)
tris(hexafluoridophosphate) acetonitrile trisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.4470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2647(16)
_cell_length_b                   14.6139(11)
_cell_length_c                   18.6288(14)
_cell_measurement_reflns_used    5333
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.57
_cell_measurement_theta_min      2.2355
_cell_volume                     5918.9(8)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2003)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25080
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.376
_diffrn_reflns_theta_min         1.679
_exptl_absorpt_coefficient_mu    2.445
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.696762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       plate
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.996
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.384(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         13146
_refine_ls_number_restraints     434
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                11295
_reflns_number_total             13146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2625sup1.cf
_cod_data_source_block           I
_cod_database_code               2020017
_shelx_estimated_absorpt_t_min   0.580
_shelx_estimated_absorpt_t_max   0.930
_shelx_hkl_checksum              71865
_shelx_res_checksum              41787
_cod_database_fobs_code 2020017