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_7040623
_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 Ce4 K8 N8 Na8 O200 W44), 9(O)'
_chemical_formula_sum            'C8 H70 B2 Ce2 K4 N4 Na4 O109 W22'
_chemical_formula_weight         6561.60
_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                 91.787(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.783(2)
_cell_length_b                   21.459(4)
_cell_length_c                   21.350(4)
_cell_measurement_reflns_used    4271
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.796
_cell_measurement_theta_min      2.215
_cell_volume                     5395.8(17)
_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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0885
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26214
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         26214
_exptl_absorpt_coefficient_mu    24.457
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0786 after correction.
The Ratio of minimum to maximum transmission is 0.5352.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    4.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5784
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.140
_refine_diff_density_min         -3.155
_refine_diff_density_rms         0.513
_refine_ls_extinction_coef       0.000054(14)
_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   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         9217
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                6502
_reflns_number_total             9217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03148j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7040623--7040628.cif.'
_cod_original_cell_volume        5395.9(17)
_cod_database_code               7040623
_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(O6) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O33)
\\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(O41) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O1W)
\\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(O36) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O13) \\sim Ueq,
Uanis(O10W) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O34) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O8W(0.5) O11W(0.5) O12W(0.5) O13W(0.5) O14W(0.5)
 Fixed Uiso: O12W(0.08772) O13W(0.08186) O14W(0.08676)
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'