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_4349238
_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         'C27 H15 Cd N O8, C2 H3 N'
_chemical_formula_sum            'C29 H18 Cd N2 O8'
_chemical_formula_weight         634.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-20
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.5139(15)
_cell_length_b                   7.2658(3)
_cell_length_c                   18.5724(8)
_cell_measurement_reflns_used    4048
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.34
_cell_measurement_theta_min      2.250
_cell_volume                     5467.1(4)
_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 0.999
_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  0.1080
_diffrn_reflns_av_unetI/netI     0.0911
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33987
_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         26.000
_diffrn_reflns_theta_min         2.011
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0590 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.8499.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       rod
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.774
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5366
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1847
_refine_ls_R_factor_gt           0.0891
_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^)+(0.0863P)^2^+31.3036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1929
_refine_ls_wR_factor_ref         0.2357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2540
_reflns_number_total             5366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02137_si_002.cif
_cod_data_source_block           4
_cod_database_code               4349238
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.828
_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
2. Restrained distances
 H32A-H25_$1
 2.1 with sigma of 0.02
 O9-C31 \\sim O6-C31 \\sim O7-C31 \\sim O8-C31
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O8) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O10) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C30) = Uanis(C26)
Uanis(C29) = Uanis(C25)
4. Rigid body (RIGU) restrains
 Cd1, Cd2, O6, O7, O8, O9, O10, O11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cd2(0.5) O6(0.33333) O7(0.33333) O8(0.6667) O9(0.6667) O10(0.5)
 O11(0.5) C22(0.33333) H22(0.33333) C23(0.33333) H23(0.33333) C25(0.33333)
 H25(0.33333) C26(0.33333) H26(0.33333) C27(0.6667) H27(0.6667) C28(0.6667)
 H28(0.6667) C29(0.6667) H29(0.6667) C30(0.6667) H30(0.6667)
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), C27(H27), C28(H28), C29(H29),
  C30(H30)
6.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C)
;
_shelx_res_checksum              61914
_shelx_hkl_checksum              32782
_shelx_fab_checksum              70920
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'