Tetraarylpyrrolo[3,2-b]pyrroles as versatile and responsive fluorescent linkers in metal-organic frameworks.
Hawes, Chris S.; Ó Máille, Gearóid M; Byrne, Kevin; Schmitt, Wolfgang; Gunnlaugsson, Thorfinnur; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10080–10092; doi:10.1039/c8dt01784k

data_7702201
_publ_section_title
;
 Tetraarylpyrrolo[3,2-b]pyrroles as versatile and responsive fluorescent
 linkers in metal-organic frameworks.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10080
_journal_page_last               10092
_journal_paper_doi               10.1039/c8dt01784k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '6(F1 Sb0.17), 0.5(C160 H144 Ag2 N16)'
_chemical_formula_sum            'C80 H72 Ag F6 N8 Sb'
_chemical_formula_weight         1489.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-01-23 deposited with the CCDC.
2018-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7985(3)
_cell_length_b                   29.4144(9)
_cell_length_c                   25.9424(8)
_cell_measurement_reflns_used    6846
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.124
_cell_measurement_theta_min      3.005
_cell_volume                     8240.1(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31802
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.435
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.966
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0877 before and 0.0701 after correction.
The Ratio of minimum to maximum transmission is 0.8211.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.626
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3737
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1770P)^2^+41.4470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2415
_refine_ls_wR_factor_ref         0.2591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3051
_reflns_number_total             3737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01784k2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               7702201
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.611
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Sb1-F4 = Sb1-F3 = Sb1-F2
 1.55 with sigma of 0.02
 Sb2-F5 = Sb2-F8 = Sb2-F6
 1.55 with sigma of 0.02
 Sb1-F3 = Sb1-F4 = Sb1-F2 = Sb1-F1
 1.6 with sigma of 0.02
 Sb2-F5 = Sb2-F8 = Sb2-F6 = Sb2-F7
 1.6 with sigma of 0.02
 F6-F5
 2.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(Sb2) \\sim Ueq, Uanis(F7) \\sim
Ueq, Uanis(F5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.01
4. Rigid body (RIGU) restrains
 Sb1, F1, F2, F3, F4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Sb2, F5, F6, F7, F8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Sb1(0.08334) F1(0.08334) F2(0.16667) F3(0.16667) F4(0.08334)
 Sb2(0.16667) F5(0.33333) F6(0.33333) F7(0.16667) F8(0.16667)
6.a 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)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              26674
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'