Contracting pore channels of a magnesium-based metal-organic framework by decorating methyl groups for effective Xe/Kr separation.
Li, Liangjun; Zhang, Xu; Xu, Wenli; Guo, Mengwei; Liu, Qingying; Li, Fangru; Liu, Tao; Xing, Tao; Li, Zhi; Wang, Mingqing; Wu, Mingbo; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5917–5921; doi:10.1039/d3dt04001a

data_7715262
_publ_section_title
;
 Contracting pore channels of a magnesium-based metal-organic framework by
 decorating methyl groups for effective Xe/Kr separation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5917
_journal_page_last               5921
_journal_paper_doi               10.1039/d3dt04001a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C57.102 H50.454 Mg4 O23.125'
_chemical_formula_sum            'C57.1 H50.46 Mg4 O23.12'
_chemical_formula_weight         1203.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-24 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.077(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.781(2)
_cell_length_b                   21.602(3)
_cell_length_c                   22.461(3)
_cell_measurement_reflns_used    2959
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.49
_cell_measurement_theta_min      2.26
_cell_volume                     7931.0(18)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker SMART APEX II diffractometer'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1131
_diffrn_reflns_av_unetI/netI     0.1282
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56887
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.396
_diffrn_reflns_theta_min         1.325
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.106
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         14520
_refine_ls_number_restraints     389
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0566P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7247
_reflns_number_total             14520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04001a2.cif
_cod_data_source_block           112004
_cod_depositor_comments          'Adding full bibliography for 7715262.cif.'
_cod_original_cell_volume        7931.2(18)
_cod_original_formula_sum        'C57.10 H50.46 Mg4 O23.12'
_cod_database_code               7715262
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.969
_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, All O(H,H) groups
2. Restrained distances
 O21A-C61A = O21-C61
 1.43 with sigma of 0.01
 O21-H21
 0.85 with sigma of 0.01
 O21A-H21A
 0.85 with sigma of 0.01
 O17A-C62A
 1.43 with sigma of 0.01
 O17A-H17D
 0.85 with sigma of 0.01
 C61A-H21A
 1.899135 with sigma of 0.02
 Mg4-H21
 2.783646 with sigma of 0.02
 Mg4-H21A
 2.668034 with sigma of 0.02
 C61-H21
 1.855427 with sigma of 0.02
 Mg3-H17D
 2.599651 with sigma of 0.02
 C62A-H17D
 1.873163 with sigma of 0.02
 Mg4-O21 \\sim Mg4-O21A
 with sigma of 0.02
 Mg3-O17A \\sim Mg3-O17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Mg1 \\sim Mg4 \\sim O19 \\sim O20 \\sim C53 \\sim C54 \\sim O20A \\sim C53A
\\sim C54A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Mg2 \\sim Mg3 \\sim O15 \\sim O16 \\sim C52 \\sim C60 \\sim O16A \\sim C52A
\\sim C60A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C24 \\sim O22 \\sim O23 \\sim O22A \\sim O23A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Mg3 \\sim O17A \\sim O17: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C45 \\sim O5 \\sim O6 \\sim O5A \\sim O6A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C50 \\sim O11 \\sim O12 \\sim O11A \\sim O12A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Mg4 \\sim O21 \\sim O21A \\sim C61 \\sim C61A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Mg3 \\sim O17A \\sim O17 \\sim C62A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O21) \\sim Ueq, Uanis(O21A) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C61A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C62A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{O15, O16A, C52A, C60A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{O15, O16, C52, C60}
{O19, O20A, C53A, C54A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{O19, O20, C53, C54}
{C24, O22A, O23A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C24, O22, O23}
{C45, O5A, O6A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C45, O5, O6}
{C50, O11A, O12A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C50, O11, O12}
5. Others
 Sof(O16A)=Sof(C52A)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(O16)=Sof(C52)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
 Sof(O20A)=Sof(C53A)=Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(2)
 Sof(O20)=Sof(C53)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2)
 Sof(O21A)=Sof(H21A)=Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(3)
 Sof(O21)=Sof(H21)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(3)
 Sof(O22A)=Sof(O23A)=1-FVAR(4)
 Sof(O22)=Sof(O23)=FVAR(4)
 Sof(O17A)=Sof(H17D)=Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(H62C)=1-FVAR(5)
 Sof(O17)=Sof(H17E)=Sof(H17F)=FVAR(5)
 Sof(O5A)=Sof(O6A)=1-FVAR(6)
 Sof(O5)=Sof(O6)=FVAR(6)
 Sof(O11A)=Sof(O12A)=1-FVAR(7)
 Sof(O11)=Sof(O12)=FVAR(7)
 Fixed Sof: O24(0.125) H24A(0.125) H24B(0.125)
6.a Riding coordinates:
 O17A(H17D), O24(H24A,H24B)
6.b Free rotating group:
 O18(H18A,H18B)
6.c Rotating group:
 O17(H17E,H17F)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C18(H18), C20(H20), C22(H22), C28(H28), C30(H30),
 C32(H32), C40(H40), C42(H42), C44(H44)
6.e Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C54(H54A,H54B,H54C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C60A(H60D,H60E,H60F),
 C54A(H54D,H54E,H54F), C61(H61A,H61B,H61C), C61A(H61D,H61E,H61F), C62A(H62A,
 H62B,H62C)
;
_shelx_res_checksum              8109
_olex2_submission_special_instructions 'No special instructions were received'