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_7235875
_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         'C60 H60 N4 O8, C H Cl3, 2(C2 H3 N)'
_chemical_formula_sum            'C65 H67 Cl3 N6 O8'
_chemical_formula_weight         1166.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-08
_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                107.657(4)
_cell_angle_beta                 95.015(3)
_cell_angle_gamma                95.481(3)
_cell_formula_units_Z            2
_cell_length_a                   13.4640(6)
_cell_length_b                   13.6873(6)
_cell_length_c                   17.0771(6)
_cell_measurement_reflns_used    6408
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.5550
_cell_measurement_theta_min      2.1010
_cell_volume                     2962.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -92.00    3.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9470  -77.0000  150.0000 95

  2 omega  -46.00   40.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -57.0000 -150.0000 86

  3 omega   -6.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408   77.0000   90.0000 42

  4 omega  -19.00   62.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -99.0000  -30.0000 81

  5 omega  -45.00   28.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408  -37.0000   60.0000 73

  6 omega   57.00   92.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0408   57.0000    0.0000 35
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0518737000
_diffrn_orient_matrix_UB_12      0.0194526000
_diffrn_orient_matrix_UB_13      0.0078946000
_diffrn_orient_matrix_UB_21      -0.0120249000
_diffrn_orient_matrix_UB_22      0.0503656000
_diffrn_orient_matrix_UB_23      0.0193480000
_diffrn_orient_matrix_UB_31      0.0028609000
_diffrn_orient_matrix_UB_32      -0.0096039000
_diffrn_orient_matrix_UB_33      0.0386309000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23583
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         26.70
_diffrn_reflns_theta_min         2.05
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         12529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+2.8594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2483
_reflns_number_gt                8192
_reflns_number_total             12529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01144b2.cif
_cod_data_source_block           2-MeCN
_cod_database_code               7235875
_chemical_oxdiff_formula         'C60 H60 N4 O8'
_chemical_oxdiff_usercomment     tte-0270314-008
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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. Others
 Fixed Sof: N22A(0.5) N22B(0.5)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28), C100(H100)
3.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C51(H51A,H51B), C61(H61A,H61B), C71(H71A,H71B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26),
 C43(H43), C44(H44), C45(H45), C46(H46), C53(H53), C54(H54), C55(H55), C56(H56),
  C63(H63), C64(H64), C65(H65), C66(H66), C73(H73), C74(H74), C75(H75), C76(H76)
3.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C300(H30D,H30E,H30F), C200(H20A,H20B,H20C)
;
_ins_header
;
TITL data_2-MeCN in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  13.464050  13.687265  17.077117 107.6574  95.0148  95.4814
ZERR    2.00   0.000578   0.000552   0.000647   0.0035   0.0033   0.0034
LATT  1
SFAC C H N O
UNIT 120.00 120.00 8.00 16.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'