Solid state halogen bonded networks vs. dynamic assemblies in solution: explaining N⋯X interactions of multivalent building blocks
Tero, Tiia-Riikka; Salorinne, Kirsi; Malola, Sami; Häkkinen, Hannu; Nissinen, Maija; CrystEngComm 17 (2015) 8231–; doi:10.1039/C5CE01144B

data_7235880
_publ_section_title
;
 Solid state halogen bonded networks vs. dynamic assemblies in solution:
 explaining N&#x22EF;X interactions of multivalent building blocks
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              8231
_journal_paper_doi               10.1039/C5CE01144B
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C6 F4 I2, C H Cl3, C30 H30 N2 O4'
_chemical_formula_sum            'C37 H31 Cl3 F4 I2 N2 O4'
_chemical_formula_weight         1003.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-01-22 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.07141(13)
_cell_length_b                   44.2970(7)
_cell_length_c                   15.7761(4)
_cell_measurement_reflns_used    19694
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.1630
_cell_measurement_theta_min      2.2840
_cell_volume                     7737.1(2)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      170.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
  1 omega  -85.00    7.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9470  -77.0000  -30.0000 184

  2 omega  -48.00   47.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9470   77.0000   90.0000 190

  3 omega    2.00   92.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408   57.0000 -150.0000 180

  4 omega   -1.00   65.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000  -90.0000 132

  5 omega  -42.00  -16.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -57.0000 -180.0000 52

  6 omega  -46.00  -11.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -57.0000   60.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0104215000
_diffrn_orient_matrix_UB_12      -0.0134079000
_diffrn_orient_matrix_UB_13      0.0234844000
_diffrn_orient_matrix_UB_21      0.0028923000
_diffrn_orient_matrix_UB_22      -0.0085551000
_diffrn_orient_matrix_UB_23      -0.0379369000
_diffrn_orient_matrix_UB_31      0.0631588000
_diffrn_orient_matrix_UB_32      -0.0018072000
_diffrn_orient_matrix_UB_33      0.0055997000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66818
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.64
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.3092
_exptl_crystal_size_mid          0.0883
_exptl_crystal_size_min          0.0615
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+17.6680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                8275
_reflns_number_total             11088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01144b2.cif
_cod_data_source_block           2-B
_cod_database_code               7235880
_chemical_oxdiff_formula         'C60 H60 N4 O8 I2 F4'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C201(H201)
2.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C2(H2), C5(H5), C12(H12), C43(H43), C45(H45), C46(H46), C44(H44),
 C53(H53), C54(H54), C56(H56), C55(H55)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C)
;
_ins_header
;
TITL 2-B in Pccn 
REM Pccn (#56, found as Pbnb in a-cb setting)
CELL 0.71073  11.071412  44.297018  15.776135  90.0000  90.0000  90.0000
ZERR    8.00   0.000133   0.000678   0.000378   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y+1/2, z 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y,-z+1/2 
SFAC C H N O F I
UNIT 480.00 480.00 32.00 64.00 32.00 16.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'