Expanding and quantifying the crystal chemistry of the flexible ligand 15aneN5
Shircliff, Anthony D.; Allbritton, Elisabeth M. A.; Davilla, Dustin J.; Gorbet, Michael-Joseph; Jones, Donald G.; Tresp, David S.; Allen, Michael B.; Shrestha, Alina; Burgess, Gwendolyn E.; Eze, John I.; Fernandez, Andrea T.; Ramirez, Daniel; Shoff, Kody J.; Crispin, Garet G.; Crone, Sarah B.; Flinn, Michael; Tran, Tien; Bryce, Darby S.; Bond, Abbagale L.; Shockey, Dylan W.; Oliver, Allen G.; Krause, Jeanette A.; Prior, Timothy J.; Hubin, Timothy J.; CrystEngComm 24 (2022) 1218–1236; doi:10.1039/D1CE01534F

data_7244204
_publ_section_title
;
 Expanding and quantifying the crystal chemistry of the flexible ligand
 15aneN5
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1218
_journal_page_last               1236
_journal_paper_doi               10.1039/D1CE01534F
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C25 H31 N3 O6 S3'
_chemical_formula_sum            'C25 H31 N3 O6 S3'
_chemical_formula_weight         565.71
_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
_audit_creation_date             2021-07-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.137(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.1713(4)
_cell_length_b                   27.181(2)
_cell_length_c                   18.8959(14)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.10
_cell_measurement_theta_min      2.354
_cell_volume                     2652.0(3)
_computing_cell_refinement       'Bruker SAINT v8.37A'
_computing_data_collection       'Bruker APEX3 v2016.1.0'
_computing_data_reduction        'Bruker SAINT v8.37A'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48221
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         31.163
_diffrn_reflns_theta_min         2.014
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8759
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS v2014.5 (Sheldrick)
 Estimated minimum and maximum transmission:  0.8759  0.9281
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.8395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5353
_reflns_number_total             6577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01534f2.cif
_cod_data_source_block           emaa02c
_cod_depositor_comments
'Adding full bibliography for 7244202--7244217.cif.'
_cod_original_cell_volume        2652.0(4)
_cod_database_code               7244204
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
1.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16), C17(H17),
 C20(H20), C21(H21), C23(H23), C24(H24)
1.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              83865
_shelx_hkl_checksum              18892
_olex2_submission_special_instructions 'No special instructions were received'