Supramolecular coordination polymers using a close to ‘V-shaped’ fluorescent 4-amino-1,8-naphthalimide Tröger’s base scaffold
Gunnlaugsson, Thorfinnur; Shanmugaraju, Sankarasekaran; Hawes, Chris Samuel; Savyasachi, A. J.; Blasco, Salvador; Kitchen, Jonathan A.; Chem. Commun.  (2017) –; doi:10.1039/C7CC07333J

data_7120827
_publ_section_title
;
 Supramolecular coordination polymers using a close to
 &#x2018;V-shaped&#x2019; fluorescent 4-amino-1,8-naphthalimide
 Tr\"oger&#x2019;s base scaffold
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC07333J
_journal_year                    2017
_chemical_formula_moiety         'C78 H52 Cd N12.5 O11, 1.5(N O3)'
_chemical_formula_sum            'C78 H55 Cd N14 O15.5'
_chemical_formula_weight         1548.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-08-14 deposited with the CCDC.
2017-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.5400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9643(8)
_cell_length_b                   26.5902(13)
_cell_length_c                   19.4124(8)
_cell_measurement_reflns_used    9111
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.016
_cell_measurement_theta_min      2.186
_cell_volume                     8366.7(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.1207
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75827
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.440
_diffrn_reflns_theta_min         1.392
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0764 before and 0.0504 after correction. The Ratio of minimum to maximum transmission is 0.7771. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             3172
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.054
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         15377
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1624
_refine_ls_R_factor_gt           0.0698
_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^)+(0.1156P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7083
_reflns_number_total             15377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07333j2.cif
_cod_data_source_block           TB_Cd_CP
_cod_original_formula_sum        'C78 H55 Cd N14 O15.50'
_cod_database_code               7120827
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.915
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{O19, O10}
3. Uiso/Uaniso restraints and constraints
Uanis(N15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O14) = Uanis(O15) = Uanis(O16) = Uanis(N15) = Uanis(O18) = Uanis(O17) =
Uanis(N14)
Uanis(O19) = Uanis(O10)
4. Rigid body (RIGU) restrains
 O9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O10, O17, O18, N14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O14, O15, O16, N15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O10(0.5) O17(0.5) O18(0.5) N14(0.5) O14(0.5) O15(0.5) O16(0.5)
 N15(0.5) O19(0.5)
6.a Free rotating group:
 O10(O17,O18,N14), O14(O15,O16,N15), O11(O12,O13,N13)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C52(H52A,
 H52B), C63(H63A,H63B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B),
 C91(H91A,H91B)
6.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29),
 C33(H33), C43(H43), C44(H44), C45(H45), C51(H51), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C66(H66), C70(H70),
 C71(H71), C72(H72), C80(H80), C86(H86), C87(H87), C88(H88), C93(H93), C94(H94),
  C95(H95), C96(H96)
;
_shelx_res_checksum              13373
_shelx_fab_checksum              23888
_olex2_submission_special_instructions 'No special instructions were received'