Synthesis and Structure of a Family of Rhodium Polystannide Clusters [Rh@Sn10]3‒, [Rh@Sn12]3‒, [Rh2@Sn17]6‒ and the First Triply-Fused Stannide, [Rh3@Sn24]5‒
Liu, Chao; Jin, Xiao; Li, Leijiao; Xu, Jun; McGrady, John E.; Sun, Zhong-Ming; Chemical Science  (2019) –; doi:10.1039/C8SC03948H

data_1550734
_publ_section_title
;
 Synthesis and Structure of a Family of Rhodium Polystannide Clusters
 [Rh@Sn10]3--, [Rh@Sn12]3--, [Rh2@Sn17]6-- and the First Triply-Fused
 Stannide, [Rh3@Sn24]5--
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03948H
_journal_year                    2019
_chemical_formula_moiety
'C26.5 H66 K4 N9.5 O6 Rh2 Sn17, C36 H72 K2 N4 O12'
_chemical_formula_sum            'C62 H140 K6 N14 O18 Rh2 Sn17'
_chemical_formula_weight         3828.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-06-02 deposited with the CCDC.    2019-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.8280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5558(14)
_cell_length_b                   16.1668(10)
_cell_length_c                   33.205(2)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      2.24
_cell_volume                     11463.7(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            70292
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.081
_diffrn_reflns_theta_min         1.580
_exptl_absorpt_coefficient_mu    4.181
_exptl_absorpt_correction_T_max  0.658
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1163 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.5077.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_description       plate
_exptl_crystal_F_000             7232
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.944
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1100
_refine_ls_number_reflns         22633
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.484
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+23.0711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19154
_reflns_number_total             22633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03948h2.cif
_cod_data_source_block           3
_cod_original_cell_volume        11463.6(12)
_cod_database_code               1550734
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C58-C61
 1.38 with sigma of 0.01
 N64-H64A
 0.7 with sigma of 0.001
3. Rigid bond restraints
 N65, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C41, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O18, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C61) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(N11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
5. Others
 Sof(C62A)=1-FVAR(1)
 Sof(C62)=FVAR(1)
 Fixed Sof: N64(0.5) N7(0.5) C63(0.5) H63A(0.5) H63B(0.5) N8(0.5) H8A(0.5)
 H8B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,
 H7B), C8(H8C,H8D), C9(H9A,H9B), C11(H11C,H11D), C12(H12A,H12B), C13(H13A,H13B),
  C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
  C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55C,H55D), C56(H56A,H56B),
  C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C2AA(H2AA,
 H2AB), C63(H63A,H63B), C0AA(H0AA,H0AB), C57(H57A,H57B), C39(H39A,H39B)
6.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B), N55(H55A,H55B), N88(H88A,H88B), N11(H11A,H11B),
 N64(H64A,H64B), N8(H8A,H8B), N65(H65A,H65B)
;
_shelx_res_checksum              99392
_olex2_submission_special_instructions 'No special instructions were received'