Guanidinium sulfates as directors of noncentrosymmetric structures
Brummel, Beau R.; Lee, Kinsey G.; Kolis, Joseph W.; Whitehead, Daniel C.; McMillen, Colin D.; CrystEngComm 23 (2021) 1643–1656; doi:10.1039/D0CE01817A

data_7242180
_publ_section_title
;
 Guanidinium sulfates as directors of noncentrosymmetric structures
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1643
_journal_page_last               1656
_journal_paper_doi               10.1039/D0CE01817A
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_sum            'C21 H87 N34 O26.5 S6'
_chemical_formula_weight         1432.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-06-26 deposited with the CCDC.	2021-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0251(8)
_cell_length_b                   22.0693(6)
_cell_length_c                   12.5545(4)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.44
_cell_volume                     7210.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            59324
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.024
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             3036
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 4541 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         13979
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0764P)^2^+3.9769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1420
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                11583
_reflns_number_total             13979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01817a1.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7242177--7242183.cif.'
_cod_original_formula_sum        'C21 H87 N34 O26.50 S6'
_cod_database_code               7242180
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              58514