Methane capture with α-cyclodextrins
Jessen, Cecilie Høgfeldt; Bendix, Jesper; Nannestad, Theis Brock; Bordallo, Heloisa N.; Pedersen, Martin Jæger; Pedersen, Christian Marcus; Bols, Mikael; New Journal of Chemistry 47 (2023) 14624–14629; doi:10.1039/D3NJ01843A

data_7062519
_publ_section_title
;
 Methane capture with \a-cyclodextrins
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14624
_journal_page_last               14629
_journal_paper_doi               10.1039/D3NJ01843A
_journal_volume                  47
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'H1.39 O, 4(H2 O), C35.85 H58.56 O29.85, C'
_chemical_formula_sum            'C36.85 H67.95 O34.84'
_chemical_formula_weight         1068.49
_chemical_name_systematic        'Cyclohexa-amylose hydrate methane complex'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-07 deposited with the CCDC.	2023-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3540(11)
_cell_length_b                   14.3606(18)
_cell_length_c                   37.141(5)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.574
_cell_measurement_theta_min      2.438
_cell_volume                     4989.1(11)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            57921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.141
_diffrn_reflns_theta_min         2.193
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1443 before and 0.0627 after correction. The Ratio of minimum to maximum transmission is 0.8789. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             2271
_exptl_crystal_preparation
'crystallized from water under methane pressure'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.856
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 6529 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         18978
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+1.3903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                16218
_reflns_number_total             18978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01843a3.cif
_cod_data_source_block           mo_d8v5624_0m_final
_cod_depositor_comments          'Adding full bibliography for 7062519.cif.'
_cod_database_code               7062519
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.964
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O35-H35A \\sim O35A-H35A
 with sigma of 0.02
 O35-H35B \\sim O35A-H35B
 with sigma of 0.02
3. Others
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(O33)=Sof(H33)=FVAR(1)
 Sof(H35A)=Sof(H35B)=FVAR(2)
 Sof(O35A)=1-FVAR(3)
 Sof(O35)=FVAR(3)
4.a Free rotating group:
 O35(H35A,H35B), O36(H36A,H36B), O29(H29A,H29B), O30(H30A,H30B)
4.b Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7A), C8(H8), C9(H9), C10(H10A),
 C11(H11), C17(H17A), C18(H18A), C19(H19), C20(H20A), C21(H21A), C22(H22A),
 C23(H23A), C24(H24A), C25(H25A), C26(H26A), C27(H27), C28(H28A), C29(H29),
 C30(H30), C32(H32), C34(H34A), C35(H35), C36(H36), C37(H37)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C13(H13A,H13B), C16(H16A,H16B), C31(H31A,H31B), C33(H33A,H33B),
 C38(H38A,H38B)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O7(H7), O10(H10), O12(H12), O14(H14), O15(H15), O17(H17), O18(H18),
 O20(H20), O21(H21), O23(H23), O24(H24), O25(H25), O26(H26), O28(H28), O33(H33)
;
_olex2_exptl_crystal_mounting_method 'silicone grease on kapton loop'
_olex2_submission_special_instructions 'No special instructions were received'