Rare earth niobate coordination polymers
Muniz, Collin N.; Patel, Hiral; Fast, Dylan B.; Rohwer, Lauren E.S.; Reinheimer, Eric W.; Dolgos, Michelle; Graham, Matt W.; Nyman, May; Journal of Solid State Chemistry 259 (2018) 48–56; doi:10.1016/j.jssc.2017.12.034

data_1561203
_publ_section_title
;
 Rare earth niobate coordination polymers
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              48
_journal_page_last               56
_journal_paper_doi               10.1016/j.jssc.2017.12.034
_journal_volume                  259
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H18 La Nb O16 S3'
_chemical_formula_sum            'C12 H18 La Nb O16 S3'
_chemical_formula_weight         746.26
_chemical_name_common
;             
'lanthanum niobyl tris-dimethylsulfoxide tris-oxalate'
;
_chemical_name_systematic
;
'lanthanum niobyl tris-dimethylsulfoxide tris-oxalate'
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_cell_angle_alpha                90
_cell_angle_beta                 97.483(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7103(6)
_cell_length_b                   14.7858(10)
_cell_length_c                   17.0221(11)
_cell_measurement_reflns_used    14127
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     2423.1(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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      100(2)
_diffrn_detector                 'Pilatus P200K HPC detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
	Number of images: 448
	           Slice: -87.0000 - 25.0000
	     Image width: 0.2500
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -82.0000
	             Phi: 108.0000
	             XTD: 30.0000
	          2theta: 3.0000
scan:
	Number of images: 385
	           Slice: -21.2500 - 75.0000
	     Image width: 0.2500
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 82.0000
	             Phi: -180.0000
	             XTD: 30.0000
	          2theta: 3.0000
scan:
	Number of images: 180
	           Slice: 48.0000 - 93.0000
	     Image width: 0.2500
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 82.0000
	             Phi: -36.0000
	             XTD: 30.0000
	          2theta: 3.0000
scan:
	Number of images: 276
	           Slice: 13.0000 - 82.0000
	     Image width: 0.2500
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 16.0000
	             Phi: -108.0000
	             XTD: 30.0000
	          2theta: 3.0000
scan:
	Number of images: 453
	           Slice: -20.2500 - 93.0000
	     Image width: 0.2500
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 82.0000
	             Phi: 144.0000
	             XTD: 30.0000
	          2theta: 3.0000
scan:
	Number of images: 260
	           Slice: -75.0000 - -10.0000
	     Image width: 0.2500
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -82.0000
	             Phi: -144.0000
	             XTD: 30.0000
	          2theta: 3.0000
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  'Rigaku XtaLABPro'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.012735
_diffrn_orient_matrix_UB_12      0.087908
_diffrn_orient_matrix_UB_13      0.053846
_diffrn_orient_matrix_UB_21      -0.020224
_diffrn_orient_matrix_UB_22      -0.035810
_diffrn_orient_matrix_UB_23      0.053679
_diffrn_orient_matrix_UB_31      0.054654
_diffrn_orient_matrix_UB_32      0.003140
_diffrn_orient_matrix_UB_33      0.022686
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22566
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.611
_diffrn_reflns_theta_min         2.525
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.541
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1456
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.022(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5317
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0288P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4977
_reflns_number_total             5317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-259-48.cif
_cod_data_source_block           test_trans
_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_sg_symbol_H-M      'C c'
_cod_database_code               1561203
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.022(14)
 -0.022(14)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S3A-O3 \\sim S3B-O3
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
C2 \\sim C1: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
C3A \\sim C3B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C4A \\sim C4B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C3A \\sim C4B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
S2B \\sim C4A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C4B \\sim C3B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C5B \\sim S3B \\sim C6B: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
S3A \\sim S3B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C6A \\sim C6B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C4B) = Uanis(C3B)
Uanis(C4A) = Uanis(C6B)
Uanis(C6A) = Uanis(C5A)
5. Rigid body (RIGU) restrains
 C6B, S3B, C5B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6A, S3A, C5A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: S3B(0.25) C4B(0.2) H4BA(0.2) H4BB(0.2) H4BC(0.2) C6B(0.25)
 H6BA(0.25) H6BB(0.25) H6BC(0.25) C3B(0.2) H3BA(0.2) H3BB(0.2) H3BC(0.2)
 C5B(0.25) H5BA(0.25) H5BB(0.25) H5BC(0.25) S2A(0.8) S2B(0.2) C3A(0.8)
 H3AA(0.8) H3AB(0.8) H3AC(0.8) C4A(0.8) H4AA(0.8) H4AB(0.8) H4AC(0.8) C5A(0.75)
 H5AA(0.75) H5AB(0.75) H5AC(0.75) S3A(0.75) C6A(0.75) H6AA(0.75) H6AB(0.75)
 H6AC(0.75)
7.a Idealised Me refined as rotating group:
 C4B(H4BA,H4BB,H4BC), C6B(H6BA,H6BB,H6BC), C3B(H3BA,H3BB,H3BC), C5B(H5BA,H5BB,
 H5BC), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,
 H4AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC)
;