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_7223113
_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 Na8 Nd4 O200 W44), O'
_chemical_formula_sum            'C4 H6 Ge2 K8 Na4 Nd2 O101 W22'
_chemical_formula_weight         6553.21
_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             2015-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-22 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.010(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.0790(7)
_cell_length_b                   12.5625(4)
_cell_length_c                   21.1756(7)
_cell_measurement_reflns_used    7249
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.180
_cell_measurement_theta_min      3.2900
_cell_volume                     4986.3(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 0.999
_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  0.1322
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_laue_measured_fraction_full 0.999
_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            62926
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.678
_diffrn_reflns_theta_max         25.678
_diffrn_reflns_theta_min         2.896
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    27.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20634
_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            purple
_exptl_crystal_density_diffrn    4.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             5692
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.328
_refine_diff_density_min         -3.574
_refine_diff_density_rms         0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         9444
_refine_ls_number_restraints     1350
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0219P)^2^+137.0457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6597
_reflns_number_total             9444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra19726k2.cif
_cod_data_source_block           rg37f
_cod_database_code               7223113
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O15, C1, C2, O42, O43, Nd1, H2A, H2B, H2C, K1, O27, O37, O38, O39, O40, O41,
 O47, O32, O20, O48, W8, W11, W7, Ge1, W2AA, W10, Na2, O11, O21, O22, O49, O31,
 O33, O34, O10, O19, O46, O13, O25, O9, O17, O18, O28, O29, O30, W6, W2, K2A,
 W9, W5, W4, W1, W3, W0AA, W1AA, K4, O12, O0AA, O2, O4, O23, O24, O7, O8, O1,
 O3, O1AA, O14, O16, O45, O44, K2B, Na3, K3, Na1, O35, O3AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, O5, Na3, O0AA
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O7, O3, O8, K3, O35, O4AA, O15
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Others
 Sof(O5)=1-FVAR(1)
 Sof(O1A)=FVAR(1)
 Fixed Sof: W4(0.06) W5(0.06) W6(0.06) O35(0.5) K2B(0.5) W1(0.94) W2(0.94)
 W3(0.94) Na1(0.5) Na2(0.5) K2A(0.5) O2AA(0.5) O4AA(0.5) O6AA(0.5) O7AA(0.5)
4.a Me refined with riding coordinates:
 C2(H2A,H2B,H2C)
;
_shelx_res_checksum              56659
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'