Shin-ichiro Noro; To be published  () –; doi:

data_3000592
_publ_section_title
;
 Structural Characterization of a Desolvated Flexible Porous Coordination
 Polymer using MicroED
;
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              438
_journal_volume                  26
_journal_year                    2026
_chemical_formula_moiety         'C27 H28 Cu F3 N4 O3 S, C F3 O3 S'
_chemical_formula_sum            'C28 H28 Cu F6 N4 O6 S2'
_chemical_formula_weight         758.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.22(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.810(3)
_cell_length_b                   17.268(4)
_cell_length_c                   10.929(4)
_cell_measurement_reflns_used    4154
_cell_measurement_temperature    79
_cell_measurement_theta_max      0.7472625083390779
_cell_measurement_theta_min      0.10645600954679486
_cell_volume                     1652.9(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      79
_diffrn_detector
'Falcon 3 direct electron camera (integration mode)'
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Transmission electron microscope'
_diffrn_measurement_method
'continuous rotation electron diffraction (MicroED)'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.2271
_diffrn_reflns_av_unetI/netI     0.2285
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            37133
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        0.781
_diffrn_reflns_theta_max         0.781
_diffrn_reflns_theta_min         0.106
_diffrn_source                   'Talos Arctica Field Emission Gun'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       powder
_exptl_crystal_F_000             265
_refine_diff_density_max         0.085
_refine_diff_density_min         -0.096
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_coef       597(24)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         4224
_refine_ls_number_restraints     340
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1441
_refine_ls_R_factor_gt           0.0875
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1051P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2169
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                1971
_reflns_number_total             4224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CuCF3SO32bpp2_response_250227.cif
_cod_data_source_block           '[Cu(CF3SO3)2(bpp)2]'
_cod_depositor_comments
'Releasing structure 3000592 into public domain as published material.'
_cod_original_cell_volume        1652.9(6)
_cod_database_code               3000592
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C6-C7 = C7-C8
 1.52 with sigma of 0.002
 C27-F1 \\sim C27-F2 \\sim C27-F3 \\sim C28-F4 \\sim C28-F5 \\sim C28-F6
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F1-F3 \\sim F4-F5 \\sim F5-F6 \\sim F4-F6
 with sigma of 0.02
 N2-C11 \\sim N2A-C11A
 with sigma of 0.02
 N2-C13 \\sim N2A-C13A
 with sigma of 0.02
 C6-C7 \\sim C6-C7A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 C9-C12 \\sim C9A-C12A
 with sigma of 0.02
 C9-C8 \\sim C9A-C8A
 with sigma of 0.02
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C12-C13 \\sim C12A-C13A
 with sigma of 0.02
 N2-C10 \\sim N2A-C10A
 with sigma of 0.04
 N2-C12 \\sim N2A-C12A
 with sigma of 0.04
 C6-C8 \\sim C6-C8A
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 C9-C11 \\sim C9A-C11A
 with sigma of 0.04
 C9-C13 \\sim C9A-C13A
 with sigma of 0.04
 C10-C12 \\sim C10A-C12A
 with sigma of 0.04
 C10-C8 \\sim C10A-C8A
 with sigma of 0.04
 C11-C13 \\sim C11A-C13A
 with sigma of 0.04
 C12-C8 \\sim C12A-C8A
 with sigma of 0.04
3. Restrained planarity
 C9, C10, C11, C12, C13, N2, C8
 with sigma of 0.1
 C8, C9, C10, C11, C12, C13, N2
 with sigma of 0.1
 C8A, C9A, C10A, C11A, C12A, C13A, N2A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F2 \\sim F3 \\sim F3 \\sim F1 \\sim F1 \\sim C27 \\sim F2
\\sim C27 \\sim F3 \\sim C27: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O1 \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
N4 \\sim C26 \\sim N4 \\sim C24: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C7A \\sim C6 \\sim C7A \\sim C8A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C9A \\sim C12A \\sim C9A \\sim C10A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N2A \\sim C13A \\sim N2A \\sim C11A \\sim N2 \\sim C13 \\sim N2 \\sim C11:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F1) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(N2)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(N4) \\sim Ueq, Uanis(N2A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C7, C7A, C8, C8A, C9, C9A, C10, C10A, C11, C11A, C12, C12A, C13, C13A, N2, N2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H6BC)=Sof(H6BD)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C11A)=
 Sof(H11A)=Sof(N2A)=1-FVAR(1)
 Sof(N2)=Sof(H6AA)=Sof(H6AB)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C9)=Sof(C10)=
 Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6AA,H6AB), C6(H6BC,H6BD), C7(H7A,H7B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C8(H8A,H8B), C7A(H7AA,H7AB), C8A(H8AA,H8AB)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C26(H26),
  C10A(H10A), C12A(H12A), C13A(H13A), C11A(H11A)
;
_shelx_res_checksum              45930
_shelx_hkl_checksum              53246
_olex2_submission_special_instructions 'No special instructions were received'