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_1563855
_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 N24 O48 Tb4), 2(C4 H9 N O), 2(C2 H8 N)'
_chemical_formula_sum            'C48 H58 Br Cu2 N10 O14 Tb'
_chemical_formula_weight         1364.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 101.707(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.920(4)
_cell_length_b                   15.464(2)
_cell_length_c                   19.388(3)
_cell_measurement_reflns_used    6521
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5554.5(17)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 49.9400
	          2theta: 29.9192
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 49.9400
	          2theta: 29.9192
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 49.9400
	          2theta: 29.9192
;
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.010365
_diffrn_orient_matrix_UB_12      -0.041646
_diffrn_orient_matrix_UB_13      0.030540
_diffrn_orient_matrix_UB_21      0.055290
_diffrn_orient_matrix_UB_22      -0.009766
_diffrn_orient_matrix_UB_23      -0.032083
_diffrn_orient_matrix_UB_31      0.033570
_diffrn_orient_matrix_UB_32      -0.001624
_diffrn_orient_matrix_UB_33      0.058347
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28516
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.577
_diffrn_reflns_theta_min         3.127
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.808
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.569
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         6402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+0.4850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5277
_reflns_number_total             6402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4.cif
_cod_data_source_block           1_pl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        5554.5(16)
_cod_database_code               1563855
_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 Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C15(H15), C18(H18)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 1563855