Exploring the self-assembly dynamics of novel steroid-coumarin conjugates: a comprehensive spectroscopic and solid-state investigation.
Ramírez-Lozano, Claudia M; Ochoa, Ma Eugenia; Labra-Vázquez, Pablo; Jiménez-Sánchez, Arturo; Farfán, Norberto; Santillan, Rosa; Organic & biomolecular chemistry 22 (2024) 3314–3327; doi:10.1039/d4ob00192c

data_7159863
_publ_section_title
;
 Exploring the self-assembly dynamics of novel steroid-coumarin
 conjugates: a comprehensive spectroscopic and solid-state investigation.
;
_journal_issue                   16
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3314
_journal_page_last               3327
_journal_paper_doi               10.1039/d4ob00192c
_journal_volume                  22
_journal_year                    2024
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C37 H54 N2 O6'
_chemical_formula_sum            'C74.18 H106.96 Cl3 N4 O13.4'
_chemical_formula_weight         1375.49
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-01-11 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                79.169(6)
_cell_angle_beta                 85.466(6)
_cell_angle_gamma                85.116(6)
_cell_formula_units_Z            1
_cell_length_a                   8.0067(18)
_cell_length_b                   10.661(2)
_cell_length_c                   23.119(5)
_cell_measurement_reflns_used    7641
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.33
_cell_measurement_theta_min      2.29
_cell_volume                     1927.2(7)
_computing_cell_refinement       'SAINT V8.38A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34535
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        20.858
_diffrn_reflns_theta_max         20.858
_diffrn_reflns_theta_min         2.291
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       plate
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.390
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 2115 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(7)
_refine_ls_extinction_coef       0.029(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         7959
_refine_ls_number_restraints     704
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0868
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1928P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2278
_refine_ls_wR_factor_ref         0.2616
_reflns_Friedel_coverage         0.980
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                5555
_reflns_number_total             7959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob00192c2.cif
_cod_data_source_block           rsclau41_0m
_cod_depositor_comments
'Adding full bibliography for 7159862--7159865.cif.'
_cod_original_cell_volume        1927.1(7)
_cod_original_formula_sum        'C74.18 H106.96 Cl3 N4 O13.40'
_cod_database_code               7159863
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              81793