First quadruple-glycine bridging mono-lanthanide-substituted borotungstate hybrids.
Liu, Jiancai; Yu, Jing; Han, Qing; Wen, Yue; Chen, Lijuan; Zhao, Junwei; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16471–16484; doi:10.1039/c6dt03148j

data_7040626
_publ_section_title
;
 First quadruple-glycine bridging mono-lanthanide-substituted
 borotungstate hybrids.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16471
_journal_page_last               16484
_journal_paper_doi               10.1039/c6dt03148j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'0.5(C16 H40 B4 K8 N8 Na8 O200 Pr4 W44), 9(O)'
_chemical_formula_sum            'C8 H70 B2 K4 N4 Na4 O109 Pr2 W22'
_chemical_formula_weight         6563.18
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-05 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7518(9)
_cell_length_b                   21.4795(16)
_cell_length_c                   21.3507(17)
_cell_measurement_reflns_used    4870
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.138
_cell_measurement_theta_min      2.220
_cell_volume                     5386.4(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27048
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         27048
_exptl_absorpt_coefficient_mu    24.559
_exptl_absorpt_correction_T_max  0.1199
_exptl_absorpt_correction_T_min  0.0839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0954 before and 0.0585 after correction. The Ratio of minimum to maximum transmission is 0.6445. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    4.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5788
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.146
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.355
_refine_ls_extinction_coef       0.000063(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         9363
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                6892
_reflns_number_total             9363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03148j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7040623--7040628.cif.'
_cod_database_code               7040626
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(B1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O8W(0.5) O9W(0.5) O11W(0.5) O13W(0.5) O14W(0.5)
 Fixed Uiso: O8W(0.08474) O13W(0.08046)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
4.b Me refined with riding coordinates:
 N1(H1C,H1D,H1E), N2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'