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_1550731
_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         'Rh Sn10, 3(C18 H36 K N2 O6), C2 H8 N2'
_chemical_formula_sum            'C56 H115 K3 N8 O18 Rh Sn10'
_chemical_formula_weight         2595.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                81.348(5)
_cell_angle_beta                 87.147(4)
_cell_angle_gamma                74.041(5)
_cell_formula_units_Z            2
_cell_length_a                   15.142(3)
_cell_length_b                   15.879(4)
_cell_length_c                   19.180(5)
_cell_measurement_reflns_used    4306
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.224
_cell_measurement_theta_min      2.189
_cell_volume                     4383.3(18)
_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)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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_unetI/netI     0.1065
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15012
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.068
_diffrn_reflns_theta_max         25.068
_diffrn_reflns_theta_min         1.348
_exptl_absorpt_coefficient_mu    3.180
_exptl_absorpt_correction_T_max  0.385
_exptl_absorpt_correction_T_min  0.237
_exptl_absorpt_correction_type   multi-scan
_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    1.967
_exptl_crystal_description       block
_exptl_crystal_F_000             2506
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.134
_refine_diff_density_min         -1.851
_refine_diff_density_rms         0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         15012
_refine_ls_number_restraints     1263
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0932P)^2^+31.8595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10615
_reflns_number_total             15012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03948h2.cif
_cod_data_source_block           1_CCDC1
_cod_original_cell_volume        4383.2(17)
_cod_database_code               1550731
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.766(2)
 0.234(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C7BA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Sn9')=Sof(Sn1')=Sof(Sn3')=1-FVAR(1)
 Sof(Sn3)=Sof(Sn9)=Sof(Sn10)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C1BA(H1BA,H1BB), C2AA(H2AA,H2AB), C2BA(H2BA,H2BB), C3BA(H3BA,
 H3BB), C4AA(H4AA,H4AB), C6AA(H6AA,H6AB), C6BA(H6BA,H6BB), C7BA(H7BA,H7BB),
 C9AA(H9AA,H9AB), C21(H21A,H21B), C24(H24A,H24B), C28(H28A,H28B), C29(H29A,
 H29B), C31(H31A,H31B), C47(H47A,H47B), C49(H49A,H49B), C52(H52A,H52B),
 C4BA(H4BA,H4BB), C5AA(H5AA,H5AB), C5BA(H5BA,H5BB), C7AA(H7AA,H7AB), C8AA(H8AA,
 H8AB), C8BA(H8BA,H8BB), C25(H25A,H25B), C30(H30A,H30B), C32(H32A,H32B),
 C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C46(H46A,H46B),
  C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C0AA(H0AA,
 H0AB), C0BA(H0BA,H0BB), C3AA(H3AA,H3AB), C22(H22A,H22B), C23(H23A,H23B),
 C26(H26A,H26B), C27(H27A,H27B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
  C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C44(H44A,H44B), C48(H48A,
 H48B), C51(H51A,H51B), C53(H53A,H53B), C58(H58A,H58B), C9BA(H9BA,H9BB),
 C43(H43A,H43B)
6.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B)
;
_shelx_res_checksum              87552
_olex2_submission_special_instructions 'No special instructions were received'