Lanthanide contraction and anion-controlled structure diversity in two types of novel 3d-4f heterometallic coordination polymers: Crystal structure and magnetic properties
Xiong, Gang; Qi, Dan; He, Yongke; You, Lixin; Ren, Baoyi; Sun, Yaguang; Inorganica Chimica Acta 483 (2018) 299–304; doi:10.1016/j.ica.2018.08.044

data_1563854
_publ_section_title
;
 Lanthanide contraction and anion-controlled structure diversity in two
 types of novel 3d-4f heterometallic coordination polymers: Crystal
 structure and magnetic properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              299
_journal_page_last               304
_journal_paper_doi               10.1016/j.ica.2018.08.044
_journal_volume                  483
_journal_year                    2018
_chemical_formula_moiety
'0.25(C144 H96 Br4 Cu8 Gd4 N24 O48), 2(C4 H9 N O), 2(C2 H8 N)'
_chemical_formula_sum            'C48 H58 Br Cu2 Gd N10 O14'
_chemical_formula_weight         1363.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 101.39(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.95(3)
_cell_length_b                   15.55(2)
_cell_length_c                   19.36(3)
_cell_measurement_reflns_used    6867
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      25.004
_cell_measurement_theta_min      3.359
_cell_volume                     5593(14)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1557
_diffrn_reflns_av_unetI/netI     0.1112
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21097
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.004
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_min         3.359
_exptl_absorpt_coefficient_mu    2.711
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.463
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         4884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0710P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4058
_reflns_number_total             4884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3.cif
_cod_data_source_block           gd_pl_pl
_cod_database_code               1563854
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.613
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C8(H8A,H8B,
 H8C), C9(H9A,H9B,H9C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 1563854