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_4349236
_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 H17 Cu N O8, 2(C3 H7 N O)'
_chemical_formula_sum            'C33 H31 Cu N3 O10'
_chemical_formula_weight         693.15
_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     direct
_audit_creation_date             2015-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                88.621(3)
_cell_angle_beta                 88.801(3)
_cell_angle_gamma                80.851(3)
_cell_formula_units_Z            2
_cell_length_a                   6.8306(9)
_cell_length_b                   10.7920(13)
_cell_length_c                   20.523(3)
_cell_measurement_reflns_used    2238
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.54
_cell_measurement_theta_min      2.17
_cell_volume                     1493.0(3)
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_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  0.0995
_diffrn_reflns_av_unetI/netI     0.1133
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21338
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.085
_diffrn_reflns_theta_min         1.912
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0623 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.8631.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         5934
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0570P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3525
_reflns_number_total             5934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02137_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        1492.9(3)
_cod_database_code               4349236
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.939
_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) groups
2. Restrained distances
 C34-N3
 1.45 with sigma of 0.01
 O11-C35
 1.2 with sigma of 0.01
 O8-H8D
 0.95 with sigma of 0.02
 H8C-O8
 0.95 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: O10(0.5) O11(0.5) C32(0.5) H32(0.5) C33(0.5) H33A(0.5) H33B(0.5)
 H33C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C35(0.5) H35(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
5.b Me refined with riding coordinates:
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
5.c 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), C32(H32), C35(H35), C28(H28)
5.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              24594
_shelx_hkl_checksum              75105
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'