Heterobimetallic [NiIILnIII] (Ln = Sm and Tb) N2O4-donor coordination polymers: Syntheses, crystal structures and fluorescence properties
Zhang, Lin-Wei; Zhang, Yu; Cui, Yong-Fan; Yu, Meng; Dong, Wen-Kui; Inorganica Chimica Acta 506 (2020) 119534–; doi:10.1016/j.ica.2020.119534

data_1564980
_publ_section_title
;
 Heterobimetallic [NiIILnIII] (Ln&#x00A0;=&#x00A0;Sm and Tb) N2O4-donor
 coordination polymers: Syntheses, crystal structures and fluorescence
 properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119534
_journal_paper_doi               10.1016/j.ica.2020.119534
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety         'C31 H33 N4 Ni O14 Tb'
_chemical_formula_sum            'C31 H33 N4 Ni O14 Tb'
_chemical_formula_weight         903.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 104.0670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8394(3)
_cell_length_b                   18.5888(4)
_cell_length_c                   17.8158(4)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.73
_cell_volume                     3482.08(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49925
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.135
_diffrn_reflns_theta_min         2.500
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.628
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+3.9877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5770
_reflns_number_total             7687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Polymer2.cif
_cod_data_source_block           190403-3_sq
_cod_database_code               1564980
_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C12(H12), C16(H16), C17(H17), C18(H18),
 C23(H23), C24(H24), C26(H26), C27(H27), C29(H29)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;