Flexible Porous Coordination Polymers from Divergent Photoluminescent 4-Oxo-1,8-naphthalimide Ligands.
Hawes, Chris S.; Byrne, Kevin; Schmitt, Wolfgang; Gunnlaugsson, Thorfinnur; Inorganic chemistry 55 (2016) 11570–11582; doi:10.1021/acs.inorgchem.6b02137

data_4349235
_publ_section_title
;
 Flexible Porous Coordination Polymers from Divergent Photoluminescent
 4-Oxo-1,8-naphthalimide Ligands.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11570
_journal_page_last               11582
_journal_paper_doi               10.1021/acs.inorgchem.6b02137
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '0.5(C108 H60 Ag2 N12 O12), B F4'
_chemical_formula_sum            'C54 H30 Ag B F4 N6 O6'
_chemical_formula_weight         1053.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.755(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.4466(4)
_cell_length_b                   39.390(3)
_cell_length_c                   31.168(2)
_cell_measurement_reflns_used    4422
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.54
_cell_measurement_theta_min      2.17
_cell_volume                     5458.7(7)
_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)'
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 8
_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       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            29855
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.223
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0684 before and 0.0607 after correction.
The Ratio of minimum to maximum transmission is 0.8025.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       rod
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5684
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0764
_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^)+(0.1342P)^2^+11.7405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3897
_reflns_number_total             5684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02137_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        5458.7(8)
_cod_database_code               4349235
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F8-F5
 2.5 with sigma of 0.02
 F8-F7
 2.5 with sigma of 0.02
 F6-F8
 2.5 with sigma of 0.02
 F7-F5
 2.5 with sigma of 0.02
 F7-F6
 2.5 with sigma of 0.02
 F6-F5
 2.5 with sigma of 0.02
 F6-B2 = F5-B2 = F7-B2
 1.4 with sigma of 0.02
 B2-F8
 1.4 with sigma of 0.02
 B1-B1_$1
 1.4 with sigma of 0.02
 F2-B1 = F4-B1 = F1-B1
 1.45 with sigma of 0.02
 F2-F1
 2.5 with sigma of 0.02
 F4-F2
 2.5 with sigma of 0.02
 F4-F1
 2.5 with sigma of 0.02
 F3-B1
 1.5 with sigma of 0.02
 F1-F3
 2.5 with sigma of 0.02
 F2-F3
 2.5 with sigma of 0.02
 F3-F4
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F7) \\sim Ueq, Uanis(B2) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of
0.04
Uanis(F2) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(B1) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F5, F6, F7, F8, B2
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 F1, F2, F3, F4, B1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: F1(0.25) F2(0.25) F3(0.25) F4(0.25) B1(0.25) F5(0.25) F6(0.25)
 F7(0.25) F8(0.25) B2(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C22(H22), C23(H23), C25(H25), C26(H26)
;
_shelx_res_checksum              31982
_shelx_hkl_checksum              76301
_shelx_fab_checksum              20975
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'