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_1563857
_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(C96 H64 Cu4 Er4 N16 O32), C4 H9 N O'
_chemical_formula_sum            'C28 H25 Cu Er N5 O9'
_chemical_formula_weight         806.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.456(14)
_cell_length_b                   24.961(16)
_cell_length_c                   12.630(8)
_cell_measurement_reflns_used    4739
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     7079(8)
_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 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.0838
	          2theta: 29.9494
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.0838
	          2theta: 29.9494
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.0838
	          2theta: 29.9494
;
_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      0.023069
_diffrn_orient_matrix_UB_12      0.075737
_diffrn_orient_matrix_UB_13      -0.001006
_diffrn_orient_matrix_UB_21      -0.035937
_diffrn_orient_matrix_UB_22      0.011262
_diffrn_orient_matrix_UB_23      0.023763
_diffrn_orient_matrix_UB_31      0.020578
_diffrn_orient_matrix_UB_32      -0.005818
_diffrn_orient_matrix_UB_33      0.033878
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15792
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.638
_diffrn_reflns_theta_min         3.069
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.007
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.820
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 1619 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4082
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+7.0012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                3601
_reflns_number_total             4082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6.cif
_cod_data_source_block           tt
_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_database_code               1563857
_shelx_estimated_absorpt_t_max   0.585
_shelx_estimated_absorpt_t_min   0.585
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2AA-O1AA
 1.28 with sigma of 0.01
 N0AA-C2AA
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N0AA \\sim C0AA \\sim C2AA \\sim C3AA \\sim O1AA \\sim C4AA: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C2AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: N0AA(0.5) O1AA(0.5) C2AA(0.5) C3AA(0.5) H3AA(0.5) H3AB(0.5)
 H3AC(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C4AA(0.5) H4AA(0.5)
 H4AB(0.5) H4AC(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C1(H1), C2(H2), C8(H8), C5(H5), C4(H4), C9(H9), C12(H12)
5.b Idealised Me refined as rotating group:
 C3AA(H3AA,H3AB,H3AC), C0AA(H0AA,H0AB,H0AC), C4AA(H4AA,H4AB,H4AC)
;
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 1563857