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_7224408
_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(C9 H7 N O), 3(C H4 O), 3(O), C32 H32 O8'
_chemical_formula_sum            'C53 H58 N2 O16'
_chemical_formula_weight         979.01
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-25
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5611(4)
_cell_length_b                   20.8203(8)
_cell_length_c                   14.9973(4)
_cell_measurement_reflns_used    4649
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      72.2550
_cell_measurement_theta_min      3.9500
_cell_volume                     5171.2(3)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega -112.00  -13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176  -57.0000  -60.0000 99

  2 omega  -72.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   77.0000 -120.0000 103

  3 omega   43.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -30.0000  -90.0000 36

  4 omega   27.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -94.0000   90.0000 78

  5 omega   77.00  171.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   30.0000  -60.0000 94

  6 omega   31.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -30.0000  150.0000 60

  7 omega  109.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  125.0000  -60.0000 30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0313120000
_diffrn_orient_matrix_UB_12      -0.0012783000
_diffrn_orient_matrix_UB_13      -0.0966243000
_diffrn_orient_matrix_UB_21      -0.0875098000
_diffrn_orient_matrix_UB_22      0.0042134000
_diffrn_orient_matrix_UB_23      0.0345018000
_diffrn_orient_matrix_UB_31      0.0043288000
_diffrn_orient_matrix_UB_32      0.0738830000
_diffrn_orient_matrix_UB_33      -0.0037629000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13761
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         66.728
_diffrn_reflns_theta_min         3.632
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83070
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.2448
_exptl_crystal_size_mid          0.0959
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         4622
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0771P)^2^+3.1897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3758
_reflns_number_total             4622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00240d2.cif
_cod_data_source_block           IsQNO_1
_cod_depositor_comments
'Adding full bibliography for 7224402--7224408.cif.'
_cod_database_code               7224408
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H20 N1 O9'
_reflns_odcompleteness_completeness 97.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 H1S-O1S
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O1W(0.25) H2S(0.5) O2W(0.5) O3W(0.125) O4W(0.125) O5W(0.25)
 O6W(0.25) H2SA(0.5) H2SB(0.5) H2SC(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14)
5.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2(H2), C4A(H4A), C5(H5), C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A),
 C9(H9), C9A(H9A), C12(H12), C15(H15), C18(H18)
5.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
5.d Idealised tetrahedral OH refined as rotating group:
 O2S(H2S), O3(H3), O11(H11), O13(H13), O17(H17)
;
_shelx_res_checksum              74306
_olex2_submission_special_instructions 'No special instructions were received'