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_7223112
_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 Sm4 W44), 4(O)'
_chemical_formula_sum            'C4 H6 Ge2 K8 Na6 O108 Sm2 W22'
_chemical_formula_weight         6723.41
_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
_cell_angle_beta                 110.760(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.2068(6)
_cell_length_b                   12.6869(3)
_cell_length_c                   21.2464(5)
_cell_measurement_reflns_used    22662
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      3.0760
_cell_measurement_theta_min      28.9770
_cell_volume                     5093.1(2)
_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  0.0715
_diffrn_reflns_av_unetI/netI     0.0440
_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            66636
_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         25.681
_diffrn_reflns_theta_min         2.880
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    26.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11698
_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            colorless
_exptl_crystal_density_diffrn    4.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.594
_refine_diff_density_min         -1.921
_refine_diff_density_rms         0.334
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         9666
_refine_ls_number_restraints     1353
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0229P)^2^+51.7855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8580
_reflns_number_total             9666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra19726k2.cif
_cod_data_source_block           rg38g
_cod_database_code               7223112
_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, Sm1, 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'