Syntheses, crystal structure, electrochemistry and luminescence properties of lanthano-germanotungstates
Gupta, Rakesh; Hussain, Firasat; Behera, Jogendra Nath; Bossoh, Amoassi Martin; Mbomekalle, Israel Martyr; Oliveira, Pedro Almeida-de; RSC Adv.  (2015) –; doi:10.1039/C5RA19726K

data_7223111
_publ_section_title
;
 Syntheses, crystal structure, electrochemistry and luminescence
 properties of lanthano-germanotungstates
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA19726K
_journal_year                    2015
_chemical_formula_moiety         '0.5(C8 H12 Ge4 K16 Na12 O208 Pr4 W44), 4(O)'
_chemical_formula_sum            'C4 H6 Ge2 K8 Na6 O108 Pr2 W22'
_chemical_formula_weight         6704.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-12 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(3)
_cell_angle_beta                 110.614(3)
_cell_angle_gamma                90.000(3)
_cell_formula_units_Z            2
_cell_length_a                   20.2680(8)
_cell_length_b                   12.7357(4)
_cell_length_c                   21.3024(7)
_cell_measurement_reflns_used    13903
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.9310
_cell_measurement_theta_min      3.1080
_cell_volume                     5146.7(3)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2013)'
_computing_data_collection       'CrysAlis RED (Oxford, 2013)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2013)'
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67150
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    26.441
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171.NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             5844
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.773
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         9763
_refine_ls_number_restraints     1353
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+61.4647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7996
_reflns_number_total             9763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra19726k2.cif
_cod_data_source_block           rg36h
_cod_database_code               7223111
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 O1, C1, C2, O42, O43, Pr1, H2A, H2B, H2C, K1, O37, O38, O39, O40, O41, O32,
 O20, W8, W11, W7, W6, W10, O11, O21, O22, K2, O31, O33, O34, O10, O19, O27,
 O54, O9, O17, O18, O25, O28, O29, O30, W3A, W2, W9, O36, O6, O12, W1A, Ge1, W1,
  W5, W4, K4, O13, W3, O2, O5, O23, O24, O4, O8, W2A, K3, O15, O16, O7, O14,
 O44, O45, O3, Na1, O35, O47, O48, O49, O50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: W1A(0.04) W2A(0.04) W3A(0.04) W1(0.96) W2(0.96) W3(0.96)
5.a Me refined with riding coordinates:
 C2(H2A,H2B,H2C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'