Eight coordination compounds assembled from unexplored semi-rigid ether-based unsymmetrical tetracarboxylate and various dipyridyl ligands: structural variation, magnetic and photoluminescence properties
Yue, Qi; Wang, Yuan-Yuan; Hu, Xiao-Lu; Guo, Wei-Xiao; Gao, En-Qing; CrystEngComm  (2019) –; doi:10.1039/C9CE01128E

data_7233975
_publ_section_title
;
 Eight coordination compounds assembled from unexplored semi-rigid
 ether-based unsymmetrical tetracarboxylate and various dipyridyl ligands:
 structural variation, magnetic and photoluminescence properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01128E
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_sum            'C80 H72 N8 Ni4 O31'
_chemical_formula_weight         1876.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2019-07-16 deposited with the CCDC.    2019-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6058(4)
_cell_length_b                   24.4866(7)
_cell_length_c                   11.6606(3)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.24
_cell_volume                     3884.84(19)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            51733
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.218
_diffrn_reflns_theta_min         1.663
_exptl_absorpt_coefficient_mu    1.051
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 3441 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                8185
_reflns_number_total             9360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01128e2.cif
_cod_data_source_block           5
_cod_database_code               7233975
_shelxl_version_number           2014-3
_shelx_res_checksum              34863