Different coordination geometries of lighter lanthanates driven by the symmetry of guanidines as charge compensators
Packiaraj, S.; Kanchana, P.; Pushpaveni, A.; Puschmann, H.; Govindarajan, S.; New Journal of Chemistry 43 (2019) 979–; doi:10.1039/C8NJ03600D

data_7058009
_publ_section_title
;
 Different coordination geometries of lighter lanthanates driven by the
 symmetry of guanidines as charge compensators
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              979
_journal_paper_doi               10.1039/C8NJ03600D
_journal_volume                  43
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H12 O12 Pr1 S3, 3(C H6 N3)'
_chemical_formula_sum            'C15 H30 N9 O12 Pr S3'
_chemical_formula_weight         765.57
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-20
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Olex2 1.2-alpha
(compiled 2012.02.15 svn.r2219, GUI svn.r4090)
;
_audit_update_record
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2012-07-11 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.8781(3)
_cell_length_b                   10.8781(3)
_cell_length_c                   15.3633(4)
_cell_measurement_reflns_used    6029
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.9639
_cell_measurement_theta_min      2.5315
_cell_volume                     1574.42(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.4 (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb 3 2012,17:36:33)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.4 (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb 3 2012,17:36:33)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.4 (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb 3 2012,17:36:33)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
1 omega -44.00 50.00 1.0000 4.3800
omega____ theta____ kappa____ phi______ frames
- -17.9366 77.0000 -120.0000 94

2 omega -8.00 27.00 1.0000 4.3800
omega____ theta____ kappa____ phi______ frames
- 18.5616 77.0000 0.0000 35

3 omega -88.00 12.00 1.0000 4.3800
omega____ theta____ kappa____ phi______ frames
- -17.9366 -77.0000 -150.0000 100

4 omega -48.00 52.00 1.0000 4.3800
omega____ theta____ kappa____ phi______ frames
- -17.9366 77.0000 -30.0000 100

5 omega -90.00 -45.00 1.0000 4.3800
omega____ theta____ kappa____ phi______ frames
- -17.9366 -38.0000 -60.0000 45

6 omega -94.00 -32.00 1.0000 4.3800
omega____ theta____ kappa____ phi______ frames
- -17.9366 179.0000 0.0000 62
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0387665000
_diffrn_orient_matrix_UB_12      0.0124100000
_diffrn_orient_matrix_UB_13      -0.0392890000
_diffrn_orient_matrix_UB_21      -0.0263247000
_diffrn_orient_matrix_UB_22      0.0442254000
_diffrn_orient_matrix_UB_23      -0.0148554000
_diffrn_orient_matrix_UB_31      0.0589439000
_diffrn_orient_matrix_UB_32      0.0596502000
_diffrn_orient_matrix_UB_33      0.0192026000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13433
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         2.54
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.811
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.4 (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb 3 2012,17:36:33)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.3789
_exptl_crystal_size_mid          0.2806
_exptl_crystal_size_min          0.2366
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1401
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+1.7754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                1218
_reflns_number_total             1401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj03600d2.cif
_cod_data_source_block           ptg3
_cod_depositor_comments
'Adding full bibliography for 7058007--7058009.cif.'
_cod_original_cell_volume        1574.40(7)
_cod_database_code               7058009
_chemical_oxdiff_formula         'C9 H14 N3 O8 Pr S2'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32