Ln polyoxocations: yttrium oxide solution speciation & solution deposited thin films.
Marsh, David A.; Goberna-Ferrón, Sara; Baumeister, Mary K.; Zakharov, Lev N.; Nyman, May; Johnson, Darren W.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 947–955; doi:10.1039/c6dt03733j

data_7041577
_publ_section_title
;
 Ln polyoxocations: yttrium oxide solution speciation &amp; solution
 deposited thin films.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              947
_journal_page_last               955
_journal_paper_doi               10.1039/c6dt03733j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C52 H156 N8 O79 S26 Y16'
_chemical_formula_sum            'C52 H156 N8 O79 S26 Y16'
_chemical_formula_weight         4413.96
_space_group_crystal_system      tetragonal
_space_group_IT_number           118
_space_group_name_Hall           'P -4 -2n'
_space_group_name_H-M_alt        'P -4 n 2'
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-18
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.11.07 svn.r3349 for OlexSys, GUI svn.r3563)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.6421(17)
_cell_length_b                   21.6421(17)
_cell_length_c                   19.6862(17)
_cell_measurement_reflns_used    6706
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.49
_cell_measurement_theta_min      2.46
_cell_volume                     9220.6(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.2074
_diffrn_reflns_av_unetI/netI     0.1077
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            107920
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.331
_exptl_absorpt_coefficient_mu    5.337
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5973
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_meas      0.17
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details
;
 Flack x determined using 1585 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.055(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         8153
_refine_ls_number_restraints     910
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1074P)^2^+77.5229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2375
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4808
_reflns_number_total             8153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03733j1.cif
_cod_data_source_block           dwj1902
_cod_depositor_comments
'Adding full bibliography for 7041576--7041577.cif.'
_cod_original_cell_volume        9220.6(17)
_cod_database_code               7041577
_shelx_estimated_absorpt_t_max   0.675
_shelx_estimated_absorpt_t_min   0.464
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 S1-C1 = S1-C2 = S2-C3 = S2-C4 = S3-C5 = S3-C6
 1.809 with sigma of 0.02
 S4-C7 = S4-C8 = S4-C8A
 1.809 with sigma of 0.02
 C7-C8 = C7-C8A
 2.75 with sigma of 0.02
 O19-C8 = O19-C8A
 2.65 with sigma of 0.02
 C20-C0AA
 2.8 with sigma of 0.001
 C16-C9
 2.82 with sigma of 0.00001
 Y5-O18B \\sim Y5-O18A
 with sigma of 0.001
 S5-O18B \\sim S6-O18A
 with sigma of 0.001
 S6-O18A \\sim O18B-S5
 with sigma of 0.001
 S6-C16 \\sim S5-C16 \\sim S6-C9 \\sim S5-C9
 with sigma of 0.0001
 S1-O15 \\sim S2-O16 \\sim S3AA-O20 \\sim S4-O19 \\sim S6-O18A \\sim S5-O18B
\\sim S3-O17 \\sim S0AA-O21
 with sigma of 0.0001
 C4-C3 \\sim C6-C5 \\sim C0AA-C20 \\sim C1-C2 \\sim C1AA-C14 \\sim C9-C16
 with sigma of 0.0001
 S3-C5 \\sim S3-C6 \\sim S3AA-C14 \\sim S3AA-C1AA \\sim S4-C8 \\sim S4-C7 \\sim
S4-C8A \\sim S5-C9 \\sim S6-C9
 \\sim S6-C16 \\sim S5-C16 \\sim S1-C2 \\sim S1-C1 \\sim S0AA-C20 \\sim
S0AA-C0AA \\sim S2-C3 \\sim S2-C4
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O18B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq, Uanis(S3AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(S0AA) \\sim Ueq, Uanis(C20) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C20) \\sim Ueq, Uanis(S0AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(S3AA) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S3, O17, C6, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O19, C8, S4, C7, C8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O21, S0AA, C20, C0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S5, O18B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O18B, S6, C16, C9, S5, Y5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
 S5, O18B, C9, C16, S6, O18A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
 O20, S3AA, C1AA, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Y3, Y1, O3, O2, O1, O10, O12, O13, O9, N2, N1, Y2, O14, O11, O6, O5, O4, Y4,
 Y5, O8, O21, O16, O7, O15, O17, O19, O20, O18A, O18B, O23, S0AA, S2, S1, S3,
 S4, S3AA, S6, S5, C0AA, C20, C3, C4, C1, C2, C5, C6, C7, C8, C8A, C1AA, C14,
 C9, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O23(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C8A(0.5) H8AA(0.5)
 H8AB(0.5) H8AC(0.5) S5(0.25) O18B(0.25) C9(0.5) H9BD(0.25) H9BE(0.25)
 H9BF(0.25) H9AA(0.25) H9AB(0.25) H9AC(0.25) C16(0.5) H16D(0.25) H16E(0.25)
 H16F(0.25) H16A(0.25) H16B(0.25) H16C(0.25) S6(0.25) O18A(0.25)
 Fixed X: C0AA(0.279869) C20(0.36357) S5(0.34375) O18B(0.30419) C9(0.425449)
 C16(0.31341) S6(0.351701) O18A(0.311251) C1AA(0.04563) C14(0.00762)
 Fixed Y: C0AA(0.522361) C20(0.621191) S5(0.87893) O18B(0.823091) C9(0.87187)
 C16(0.912809) S6(0.842381) O18A(0.809429) C1AA(0.91383) C14(0.79848)
 Fixed Z: C0AA(0.482659) C20(0.498409) S5(0.8331) O18B(0.82789) C9(0.85309)
 C16(0.91074) S6(0.883141) O18A(0.83418) C1AA(0.58006) C14(0.528181)
6.a Riding coordinates:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C0AA(H0AA,H0AB,H0AC), C20(H20A,H20B,
 H20C), C1AA(H1AA,H1AB,H1AC), C14(H14A,H14B,H14C)
6.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9BD,H9BE,H9BF), C9(H9AA,H9AB,
 H9AC), C16(H16D,H16E,H16F), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              27313
_shelx_hkl_checksum              79237
_shelx_fab_checksum              19053
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'