Structural chemistry and environment-dependent fluorescence of a tetratopic pyrrolo[3,2-b]pyrrole ligand
Brown, Corey L.; Elliott, Scarlett H.; Woodfine, Sian E.; Hawes, Chris S.; CrystEngComm 27 (2025) 7358–7366; doi:10.1039/D5CE00926J

data_7251122
_publ_section_title
;
 Structural chemistry and environment-dependent fluorescence of a
 tetratopic pyrrolo[3,2-b]pyrrole ligand
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              7358
_journal_page_last               7366
_journal_paper_doi               10.1039/D5CE00926J
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C36 H28 N2 O11 Sr2, 1.75(C H4 O), H2 O'
_chemical_formula_sum            'C37.75 H37 N2 O13.75 Sr2'
_chemical_formula_weight         913.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-09-14 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                72.2970(10)
_cell_angle_beta                 81.9980(10)
_cell_angle_gamma                82.6190(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1771(5)
_cell_length_b                   13.2036(6)
_cell_length_c                   14.7842(6)
_cell_measurement_reflns_used    7457
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      18.11
_cell_measurement_theta_min      3.21
_cell_volume                     2233.05(16)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43514
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.287
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.449
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0725 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.8730.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             927
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.804
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         9247
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0845P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6078
_reflns_number_total             9247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00926j2.cif
_cod_data_source_block           Sr2L1-MeOH
_cod_depositor_comments
'Adding full bibliography for 7251119--7251122.cif.'
_cod_database_code               7251122
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.653
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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
 H14-O3_$1
 1.958 with sigma of 0.01
 H12A-O13_$2
 2.14 with sigma of 0.02
 O4-H12B
 1.96 with sigma of 0.02
 O13-C37
 1.47 with sigma of 0.01
3. Others
 Fixed Sof: O13(0.75) H13A(0.75) C37(0.75) H37A(0.75) H37B(0.75) H37C(0.75)
4.a Free rotating group:
 O12(H12A,H12B)
4.b Rotating group:
 O9(H9A,H9B), O11(H11A,H11B), O10(H10A,H10B)
4.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C17(H17A,H17B)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C6(H6), C22(H22), C9(H9), C23(H23), C32(H32),
 C13(H13), C35(H35), C31(H31), C16(H16), C34(H34), C28(H28), C26(H26), C25(H25),
  C12(H12), C15(H15)
4.e Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C37(H37A,H37B,H37C)
4.f Idealised tetrahedral OH refined as rotating group:
 O14(H14), O13(H13A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 137 electrons were 
found in a volume of 397\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3.5[CH3OH] per Formula Unit 
which account for 126 electrons 
per unit cell. This material is a solvent-exchanged 
species which rapidly loses solvent when removed from 
the exchange media; it is not possible to quantify the 
total solvation in the fresh material
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75713
_shelx_fab_checksum              25773
_olex2_submission_special_instructions 'No special instructions were received'