Conformational changes in Cmethyl-resorcinarene pyridine N-oxide inclusion complexes in the solid state
Puttreddy, Rakesh; Beyeh, Ngong Kodiah; Rissanen, Kari; CrystEngComm 18 (2016) 4971–; doi:10.1039/C6CE00240D

data_7224403
_publ_section_title
;
 Conformational changes in Cmethyl-resorcinarene pyridine N-oxide
 inclusion complexes in the solid state
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4971
_journal_paper_doi               10.1039/C6CE00240D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '2(C6 H7 N O), C32 H32 O8'
_chemical_formula_sum            'C44 H46 N2 O10'
_chemical_formula_weight         762.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-28 deposited with the CCDC.
2016-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                113.562(7)
_cell_angle_beta                 94.266(6)
_cell_angle_gamma                90.364(6)
_cell_formula_units_Z            2
_cell_length_a                   9.9521(7)
_cell_length_b                   13.7594(10)
_cell_length_c                   15.1539(12)
_cell_measurement_reflns_used    3155
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.2270
_cell_measurement_theta_min      3.5260
_cell_volume                     1895.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -48.00   46.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1368   77.0000  120.0000 94

  2 omega    9.00   48.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1368   77.0000  150.0000 39

  3 omega  -46.00   28.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1368   77.0000   30.0000 74

  4 omega  -26.00   48.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1368   77.0000 -120.0000 74

  5 omega   -9.00   35.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2305   77.0000    0.0000 44

  6 omega  -11.00   34.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2305   77.0000 -120.0000 45
;
_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      -0.0493178000
_diffrn_orient_matrix_UB_12      0.0371119000
_diffrn_orient_matrix_UB_13      0.0217761000
_diffrn_orient_matrix_UB_21      -0.0274494000
_diffrn_orient_matrix_UB_22      -0.0052708000
_diffrn_orient_matrix_UB_23      -0.0463198000
_diffrn_orient_matrix_UB_31      -0.0439331000
_diffrn_orient_matrix_UB_32      -0.0419845000
_diffrn_orient_matrix_UB_33      -0.0025063000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12446
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.943
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0549P)^2^+0.1289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4730
_reflns_number_total             6848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00240d2.cif
_cod_data_source_block           3MePyNO_1
_cod_depositor_comments
'Adding full bibliography for 7224402--7224408.cif.'
_cod_database_code               7224403
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H20 N1 O9'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C2(H2), C2A(H2A), C2B(H2B), C3A(H3A), C3B(H3B), C5(H5),
 C5A(H5A), C5B(H5B), C9(H9), C12(H12), C16(H16), C23(H23), C26(H26)
2.c Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C6B(H6BA,H6BB,H6BC), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
2.d Idealised tetrahedral OH refined as rotating group:
 O11(H11), O20(H20)
;
_shelx_res_checksum              30844
_olex2_submission_special_instructions 'No special instructions were received'