A pseudo-icosahedral cage {Gd12} based on aminomethylphosphonate.
Zhang, Ze-Min; Zangana, Karzan H.; Kostopoulos, Andreas K.; Tong, Ming-Liang; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9041–9044; doi:10.1039/c6dt00876c

data_7039243
_publ_section_title
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 A pseudo-icosahedral cage {Gd12} based on aminomethylphosphonate.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9041
_journal_page_last               9044
_journal_paper_doi               10.1039/c6dt00876c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C132 H222 Gd12 N12 O90 P12, Co H12 O6, 18(H2 O) 4(H16 C6 N) 8(H3 C2 N)'
_chemical_formula_sum            'C172 H418 Co Gd12 N24 O114 P12'
_chemical_formula_weight         6964.85
_chemical_name_common            Gd12
_chemical_name_systematic        Gd12
_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_Hall           '-P 4c 2'
_space_group_name_H-M_alt        'P 42/m m c'
_symmetry_space_group_name_Hall  '-P 4c 2'
_symmetry_space_group_name_H-M   'P 42/m m c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-04-14 deposited with the CCDC.
2016-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.0168(10)
_cell_length_b                   28.0168(10)
_cell_length_c                   21.7936(7)
_cell_measurement_reflns_used    7213
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.8230
_cell_measurement_theta_min      3.4520
_cell_volume                     17106.7(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35717
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.349
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.220
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       prism
_exptl_crystal_F_000             7010
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.190
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         8391
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.0803
_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^)+(0.1260P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2343
_refine_ls_wR_factor_ref         0.2654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3553
_reflns_number_total             8391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00876c2.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 7039243.cif.'
_cod_original_cell_volume        17106.7(13)
_cod_database_code               7039243
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C5 = C5-C7
 1.52 with sigma of 0.02
 C8-C5 = C5-C6
 1.52 with sigma of 0.02
 C7-C5 = C5-C8
 1.52 with sigma of 0.02
 C17-C15 = C15-C16
 1.52 with sigma of 0.02
 C18-C15 = C15-C17
 1.52 with sigma of 0.02
 C18-C15 = C15-C16
 1.52 with sigma of 0.02
 C14-C15 = C15-C16
 1.52 with sigma of 0.02
 C14-C15 = C15-C17
 1.52 with sigma of 0.02
 C14-C15 = C15-C18
 1.52 with sigma of 0.02
 O13-C14 = C14-O14
 1.25 with sigma of 0.02
 O7-C4 = C4-O8
 1.25 with sigma of 0.02
 O11-C9 = C9-O10
 1.25 with sigma of 0.02
 C9-C10
 1.53 with sigma of 0.02
 C4-C5
 1.53 with sigma of 0.02
 C7-C5 = C5-C4
 1.52 with sigma of 0.02
 C6-C5 = C5-C4
 1.52 with sigma of 0.02
 C8-C5 = C5-C4
 1.52 with sigma of 0.02
 C13-C10 = C10-C11
 1.52 with sigma of 0.02
 C11-C10 = C10-C12
 1.52 with sigma of 0.02
 C12-C10 = C10-C13
 1.52 with sigma of 0.02
 C9-C10
 1.52 with sigma of 0.02
 C9-C10 = C10-C13
 1.52 with sigma of 0.02
 C9-C10 = C10-C12
 1.52 with sigma of 0.02
 P1-C1
 1.8 with sigma of 0.02
 P2-C2
 1.8 with sigma of 0.02
 P3-C3
 1.8 with sigma of 0.02
 C1-N1
 1.47 with sigma of 0.02
 C1-N5
 1.47 with sigma of 0.02
 C2-N2
 1.47 with sigma of 0.02
 C2-N6
 1.47 with sigma of 0.02
 C3-N3
 1.47 with sigma of 0.02
 C3-N4
 1.47 with sigma of 0.02
 C6-C7
 2.49 with sigma of 0.04
 C8-C6
 2.49 with sigma of 0.04
 C7-C8
 2.49 with sigma of 0.04
 C17-C16
 2.49 with sigma of 0.04
 C18-C17
 2.49 with sigma of 0.04
 C18-C16
 2.49 with sigma of 0.04
 C14-C16
 2.49 with sigma of 0.04
 C14-C17
 2.49 with sigma of 0.04
 C14-C18
 2.49 with sigma of 0.04
 O13-O14
 2.165 with sigma of 0.04
 O7-O8
 2.165 with sigma of 0.04
 O11-O10
 2.165 with sigma of 0.04
 C7-C4
 2.49 with sigma of 0.04
 C6-C4
 2.49 with sigma of 0.04
 C8-C4
 2.49 with sigma of 0.04
 C13-C11
 2.49 with sigma of 0.04
 C11-C12
 2.49 with sigma of 0.04
 C12-C13
 2.49 with sigma of 0.04
 O10-C10
 2.38 with sigma of 0.04
 O11-C10
 2.38 with sigma of 0.04
 C9-C13
 2.49 with sigma of 0.04
 C9-C12
 2.49 with sigma of 0.04
 O14-C15
 2.45 with sigma of 0.04
 O13-C15
 2.45 with sigma of 0.04
 O13-C15
 2.45 with sigma of 0.02
 O14-C15
 2.45 with sigma of 0.02
 O11-C10
 2.45 with sigma of 0.02
 O10-C10
 2.45 with sigma of 0.02
 P1-N1
 2.7 with sigma of 0.02
 P1-N5
 2.7 with sigma of 0.02
 P2-N2
 2.7 with sigma of 0.02
 P2-N6
 2.7 with sigma of 0.02
 P3-N3
 2.7 with sigma of 0.02
 P3-N4
 2.7 with sigma of 0.02
3. Rigid bond restraints
 Gd1, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Gd1, O8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Gd2, O5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Gd2, O11
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Gd2, C9
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 P1, O2
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 P2, O3
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 P3, O5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O7, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O8, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C9, O10
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C9, O11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C5
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C10, C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O14, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
C4: within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.005
C9: within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.005
O11: within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.005
O5: within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.005
C1 \\sim C2 \\sim C15 \\sim C16 \\sim C3 \\sim C9 \\sim C18 \\sim C14 \\sim C5
\\sim C7 \\sim C4 \\sim C6 \\sim C8 \\sim C17 \\sim C10 \\sim C11 \\sim C12
\\sim C13: within 1.6A with sigma of 0.01 and sigma for terminal atoms of 0.02
O5 \\sim O3 \\sim O2 \\sim O6 \\sim O1 \\sim O4 \\sim O9 \\sim O12 \\sim O17
\\sim O7 \\sim O10 \\sim O14 \\sim O8 \\sim O13 \\sim O11 \\sim O15 \\sim O16:
within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: N6(0.33333) N1(0.16667) O16(0.75) H16D(0.75) H16E(0.75)
 N2(0.16667) N4(0.33333) N3(0.16667) N5(0.33333)
6.a Riding coordinates:
 O17(H17D,H17E), O16(H16D,H16E)
6.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C),
 C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
  C13(H13A,H13B,H13C)
6.c Aromatic/amide H refined with riding coordinates:
 O9(H9), O12(H12), O15(H15)
;
_shelx_res_checksum              50824
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'