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_7042094
_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
'3(C24 H20 As), C6 Fe N6, C18 N12, O, 2(C2 H3 N)'
_chemical_formula_sum            'C100 H66 As3 Fe N20 O'
_chemical_formula_weight         1844.33
_chemical_properties_physical    ', Air-sensitive'
_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
_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                 122.3080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9359(4)
_cell_length_b                   27.5973(6)
_cell_length_c                   17.7530(6)
_cell_measurement_reflns_used    18845
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.50
_cell_volume                     8669.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      120.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_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  0.0694
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40105
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.238
_diffrn_reflns_theta_min         2.952
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0721 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.8372.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             3756
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 5214 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         16750
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0219P)^2^+8.6898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                13719
_reflns_number_total             16750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00293a2.cif
_cod_data_source_block           jk003a-auto
_cod_depositor_comments
'Adding full bibliography for 7042093--7042096.cif.'
_cod_database_code               7042094
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.446
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.521(9) 0.479(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C87(H87), C88(H88), C92(H92), C89(H89), C41(H41), C38(H38), C54(H54),
 C76(H76), C45(H45), C42(H42), C95(H95), C93(H93), C44(H44), C78(H78), C60(H60),
  C66(H66), C47(H47), C68(H68), C26(H26), C64(H64), C58(H58), C75(H75),
 C71(H71), C30(H30), C82(H82), C27(H27), C70(H70), C74(H74), C36(H36), C56(H56),
  C53(H53), C72(H72), C62(H62), C83(H83), C86(H86), C51(H51), C50(H50),
 C32(H32), C35(H35), C84(H84), C63(H63), C48(H48), C65(H65), C28(H28), C46(H46),
  C40(H40), C90(H90), C34(H34), C29(H29), C39(H39), C59(H59), C77(H77),
 C96(H96), C80(H80), C94(H94), C57(H57), C33(H33), C52(H52), C81(H81), C69(H69)
3.b Idealised Me refined as rotating group:
 C100(H10A,H10B,H10C), C98(H98A,H98B,H98C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'