Aromatic N-oxide templates open inclusion and dimeric capsular assemblies with methylresorcinarene
Beyeh, Ngong Kodiah; Puttreddy, Rakesh; Rissanen, Kari; RSC Advances 5 (2015) 30222–; doi:10.1039/C5RA03667D

data_7235903
_publ_section_title
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 Aromatic N-oxide templates open inclusion and dimeric capsular assemblies
 with methylresorcinarene
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              30222
_journal_paper_doi               10.1039/C5RA03667D
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C40 H48 O8, C9 H7 N O, 3(C H4 O)'
_chemical_formula_sum            'C52 H67 N O12'
_chemical_formula_weight         898.06
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-02-27 deposited with the CCDC.
2015-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                95.58(3)
_cell_angle_beta                 106.88(3)
_cell_angle_gamma                113.40(3)
_cell_formula_units_Z            2
_cell_length_a                   12.143(2)
_cell_length_b                   12.791(3)
_cell_length_c                   18.158(4)
_cell_measurement_temperature    170
_cell_volume                     2403.2(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.1182
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22981
_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         25.250
_diffrn_reflns_theta_min         1.976
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0834 before and 0.0732 after correction.
The Ratio of minimum to maximum transmission is 0.8565.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       needle
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8696
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0315P)^2^+2.1478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4816
_reflns_number_total             8696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra03667d2.cif
_cod_data_source_block           3_2@1_2(CH3OH)6
_cod_original_cell_volume        2403.1(10)
_cod_database_code               7235903
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.028) H7A(0.044) H7B(0.044) H7C(0.044) H8A(0.033) H9A(0.044)
 H9B(0.044) H10A(0.094) H10B(0.094) H10C(0.094) H16(0.03) H17A(0.061)
 H17B(0.061) H17C(0.061) H18(0.027) H19A(0.034) H19B(0.034) H20A(0.065)
 H20B(0.065) H20C(0.065) H25(0.026) H27A(0.044) H27B(0.044) H27C(0.044)
 H28(0.025) H29A(0.03) H29B(0.03) H30A(0.052) H30B(0.052) H30C(0.052)
 H36(0.023) H37A(0.042) H37B(0.042) H37C(0.042) H38(0.027) H39A(0.035)
 H39B(0.035) H40A(0.066) H40B(0.066) H40C(0.066) H41(0.046) H42(0.049)
 H43(0.043) H46(0.044) H47(0.051) H48(0.051) H49(0.042) H51A(0.154) H51B(0.154)
 H51C(0.154) H50A(0.081) H50B(0.081) H50C(0.081) H52A(0.087) H52B(0.087)
 H52C(0.087)
 Fixed X: H6A(0.2206) H7A(0.4947) H7B(0.53) H7C(0.3981) H8A(0.019) H9A(-
 0.1139) H9B(0.0114) H10A(-0.0694) H10B(-0.0528) H10C(0.0713) H16(0.0362)
 H17A(0.0142) H17B(0.0192) H17C(-0.1153) H18(-0.0689) H19A(-0.0913) H19B(-
 0.039) H20A(-0.2692) H20B(-0.2687) H20C(-0.22) H25(0.1664) H27A(0.3782)
 H27B(0.2315) H27C(0.3247) H28(0.4493) H29A(0.3707) H29B(0.2516) H30A(0.1864)
 H30B(0.2952) H30C(0.177) H36(0.3531) H37A(0.8697) H37B(0.8326) H37C(0.8042)
 H38(0.5394) H39A(0.3438) H39B(0.3018) H40A(0.3849) H40B(0.5178) H40C(0.4761)
 H41(0.4351) H42(0.3877) H43(0.3335) H46(0.2968) H47(0.2883) H48(0.3274)
 H49(0.381) H51A(0.7318) H51B(0.8425) H51C(0.7221) H50A(0.0899) H50B(0.2254)
 H50C(0.1242) H52A(0.7131) H52B(0.7743) H52C(0.7313)
 Fixed Y: H6A(0.1296) H7A(0.1238) H7B(0.0446) H7C(-0.0125) H8A(-0.0068) H9A(-
 0.0396) H9B(0.0229) H10A(-0.1833) H10B(-0.1898) H10C(-0.1276) H16(0.2012)
 H17A(0.4031) H17B(0.2875) H17C(0.2831) H18(0.4245) H19A(0.3584) H19B(0.2662)
 H20A(0.1796) H20B(0.2592) H20C(0.1607) H25(0.3872) H27A(0.8478) H27B(0.8249)
 H27C(0.87) H28(0.6006) H29A(0.4246) H29B(0.3653) H30A(0.428) H30B(0.5595)
 H30C(0.5023) H36(0.3092) H37A(0.6245) H37B(0.5744) H37C(0.6802) H38(0.172)
 H39A(0.027) H39B(0.1274) H40A(0.0793) H40B(0.1117) H40C(0.2125) H41(0.622)
 H42(0.425) H43(0.3053) H46(0.2838) H47(0.3672) H48(0.5637) H49(0.6796)
 H51A(0.8457) H51B(0.9621) H51C(0.967) H50A(0.7738) H50B(0.8019) H50C(0.6689)
 H52A(0.9485) H52B(1.0312) H52C(1.0808)
 Fixed Z: H6A(0.1528) H7A(0.4639) H7B(0.4101) H7C(0.426) H8A(0.2588)
 H9A(0.1257) H9B(0.1037) H10A(0.0669) H10B(0.1568) H10C(0.1337) H16(0.1407)
 H17A(0.4234) H17B(0.4474) H17C(0.3966) H18(0.1462) H19A(0.014) H19B(0.0405)
 H20A(-0.0175) H20B(0.0565) H20C(0.0697) H25(0.0817) H27A(0.2721) H27B(0.2353)
 H27C(0.1865) H28(0.0629) H29A(-0.0328) H29B(-0.0048) H30A(-0.1195) H30B(-
 0.0766) H30C(-0.0474) H36(0.0842) H37A(0.2631) H37B(0.3344) H37C(0.3092)
 H38(0.1779) H39A(0.0792) H39B(0.0587) H40A(-0.0335) H40B(0.0363) H40C(0.0159)
 H41(0.2862) H42(0.2513) H43(0.3354) H46(0.4644) H47(0.5794) H48(0.6076)
 H49(0.5211) H51A(0.3835) H51B(0.4483) H51C(0.3855) H50A(0.4119) H50B(0.4775)
 H50C(0.4323) H52A(0.1869) H52B(0.2745) H52C(0.1992)
;
_shelx_res_checksum              75532
_shelx_hkl_checksum              97274
_olex2_submission_special_instructions 'No special instructions were received'