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_7251120
_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         'C42 H38 N4 O11 Sr2, C3 H7 N O, O'
_chemical_formula_sum            'C45 H47 N5 O13 Sr2'
_chemical_formula_weight         1041.11
_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                73.6540(10)
_cell_angle_beta                 81.6760(10)
_cell_angle_gamma                84.4280(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1393(4)
_cell_length_b                   13.1440(4)
_cell_length_c                   15.0291(4)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      30.369
_cell_measurement_theta_min      2.683
_cell_volume                     2272.84(12)
_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 0.995
_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  0.0674
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            74832
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         2.314
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.417
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0629 before and 0.0532 after correction.
The Ratio of minimum to maximum transmission is 0.8518.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.072
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         13882
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0656P)^2^+2.6519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9771
_reflns_number_total             13882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00926j2.cif
_cod_data_source_block           Sr2L1
_cod_depositor_comments
'Adding full bibliography for 7251119--7251122.cif.'
_cod_database_code               7251120
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.698
_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 C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N4-C45 \\sim N5-C45 \\sim N4-C46 \\sim N4-C47 \\sim N5-C47 \\sim N5-C48
 with sigma of 0.02
 Sr1-H10A \\sim Sr1-H10B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C40) = Uanis(C43)
4. Rigid body (RIGU) restrains
 C45, C47, N4, C46, N5, C48
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O11, C43, N7, C42, C44, C40, N6, C41
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: H42A(0.5) H42B(0.5) H42C(0.5) H42D(0.5) H42E(0.5) H42F(0.5)
 N6(0.5) C40(0.5) H40(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) N7(0.5)
 C43(0.5) H43(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) H45(0.5) H45A(0.5)
 H47A(0.5) H47B(0.5) H47C(0.5) H47D(0.5) H47E(0.5) H47F(0.5) N4(0.5) C46(0.5)
 H46A(0.5) H46B(0.5) H46C(0.5) N5(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5)
 O13(0.5) O15(0.5)
6.a Free rotating group:
 O10(H10A,H10B)
6.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C20(H20A,H20B)
6.c Me refined with riding coordinates:
 C42(H42A,H42B,H42C), C42(H42D,H42E,H42F), C41(H41A,H41B,H41C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C31(H31), C32(H32),
  C34(H34), C35(H35), C37(H37), C40(H40), C43(H43), C45(H45), C45(H45A)
6.e Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C47(H47A,H47B,H47C), C47(H47D,H47E,
 H47F)
;
_shelx_res_checksum              52446
_olex2_submission_special_instructions 'No special instructions were received'