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_1564979
_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         'C70 H70 N6 Ni2 O26 Sm2, C H4 O'
_chemical_formula_sum            'C71 H74 N6 Ni2 O27 Sm2'
_chemical_formula_weight         1861.48
_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   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                82.5070(10)
_cell_angle_beta                 84.7850(10)
_cell_angle_gamma                71.3950(10)
_cell_formula_units_Z            1
_cell_length_a                   10.1047(3)
_cell_length_b                   11.8404(3)
_cell_length_c                   17.8701(5)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.137
_cell_measurement_theta_min      2.736
_cell_volume                     2006.24(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31299
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.136
_diffrn_reflns_theta_max         25.136
_diffrn_reflns_theta_min         2.736
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.984
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       block
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7106
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0414P)^2^+2.0806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6092
_reflns_number_total             7106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Polymer1.cif
_cod_data_source_block           3_sq
_cod_database_code               1564979
_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 O(H) groups
2. Restrained distances
 O13-C36
 1.43 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) O13(0.5) H13(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C19(H19A,H19B), C10(H10A,H10B), C11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C27(H27), C8(H8), C28(H28), C12(H12), C6(H6), C33(H33), C24(H24),
 C16(H16), C7(H7), C18(H18), C23(H23), C17(H17), C31(H31), C32(H32)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C20(H20A,H20B,
 H20C), C36(H36A,H36B,H36C)
5.d Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_shelx_res_checksum              7283
_shelx_hkl_checksum              13021
_shelx_fab_checksum              85649
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'