Anion-π recognition between [M(CN)6](3-) complexes and HAT(CN)6: structural matching and electronic charge density modification.
Kobylarczyk, Jedrzej; Pinkowicz, Dawid; Srebro-Hooper, Monika; Hooper, James; Podgajny, Robert; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3482–3491; doi:10.1039/c7dt00293a

data_7042093
_publ_section_title
;
 Anion-\p recognition between [M(CN)6](3-) complexes and HAT(CN)6:
 structural matching and electronic charge density modification.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3482
_journal_page_last               3491
_journal_paper_doi               10.1039/c7dt00293a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C6 Fe1 N6, 3(C24 H20 P), C18 N12'
_chemical_formula_sum            'C96 H60 Fe N18 P3'
_chemical_formula_weight         1614.38
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-09 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   27.6091(8)
_cell_length_b                   27.6091(8)
_cell_length_c                   18.7133(7)
_cell_measurement_reflns_used    6854
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      3.13
_cell_volume                     12353.4(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.1
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.363
_diffrn_reflns_theta_min         3.134
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0547 before and 0.0504 after correction.
The Ratio of minimum to maximum transmission is 0.9125.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       needle
_exptl_crystal_F_000             4998
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 711 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(16)
_refine_ls_extinction_coef       0.00027(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         3369
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0353P)^2^+7.2849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3132
_reflns_number_total             3369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00293a2.cif
_cod_data_source_block           jk001_dp_xprep-auto
_cod_depositor_comments
'Adding full bibliography for 7042093--7042096.cif.'
_cod_original_cell_volume        12353.4(9)
_cod_database_code               7042093
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.889
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.99(3) 0.01(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C29(H29), C28(H28), C20(H20), C19(H19), C18(H18), C24(H24),
 C23(H23), C22(H22), C31(H31), C32(H32), C10(H10), C11(H11), C12(H12), C13(H13),
  C14(H14), C17(H17), C16(H16), C26(H26), C25(H25)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'