Stable thiolate adducts of Rh<sub>2</sub>(OAc)<sub>4</sub> - assembly of hexametallic Ni<sub>4</sub>Rh<sub>2</sub> complexes.
Schmorl, Sara; Börner, Martin; Kersting, Berthold; Dalton transactions (Cambridge, England : 2003) 51 (2021) 59–62; doi:10.1039/d1dt03509f

data_7708952
_publ_section_title
;
 Stable thiolate adducts of Rh<sub>2</sub>(OAc)<sub>4</sub> - assembly of
 hexametallic Ni<sub>4</sub>Rh<sub>2</sub> complexes.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              59
_journal_page_last               62
_journal_paper_doi               10.1039/d1dt03509f
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety
'2(C42 H70 F N6 Ni2 O4 Rh S2), 2(Cl O4), 4(C3 H7 N O)'
_chemical_formula_sum            'C96 H168 Cl2 F2 N16 Ni4 O20 Rh2 S4'
_chemical_formula_weight         2544.25
_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'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc28zp21
_audit_creation_date             2021-10-05
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-11-12 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.3780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.5460(2)
_cell_length_b                   18.12490(10)
_cell_length_c                   27.9275(2)
_cell_measurement_reflns_used    141607
_cell_measurement_temperature    180
_cell_measurement_theta_max      71.11
_cell_measurement_theta_min      3.04
_cell_volume                     12271.44(16)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.144.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.00
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
 3950 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            147300
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.767
_diffrn_reflns_theta_min         3.183
_exptl_absorpt_coefficient_mu    4.387
_exptl_absorpt_correction_T_max  0.0219
_exptl_absorpt_correction_T_min  0.0029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5336
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.313
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1385
_refine_ls_number_reflns         23253
_refine_ls_number_restraints     361
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0794P)^2^+3.2886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18645
_reflns_number_total             23253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03509f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7708952.cif.'
_cod_database_code               7708952
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.341
_shelx_estimated_absorpt_t_min   0.255
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N15-C94
 1.46 with sigma of 0.02
 C96-O19
 1.22 with sigma of 0.02
 C96-N15
 1.36 with sigma of 0.02
 N15-C95
 1.45 with sigma of 0.02
 N13-C88
 1.46 with sigma of 0.02
 C90-N13
 1.36 with sigma of 0.02
 N13-C89
 1.45 with sigma of 0.02
 C90-O17
 1.22 with sigma of 0.02
 C96-C94
 2.45 with sigma of 0.04
 C96-C95
 2.46 with sigma of 0.04
 C90-C89
 2.46 with sigma of 0.04
 C90-C88
 2.45 with sigma of 0.04
 C73-C74 \\sim C73-C76 \\sim C73-C75
 with sigma of 0.02
 Cl2A-O13A \\sim Cl2A-O14A \\sim Cl2A-O15A \\sim Cl2A-O16A
 with sigma of 0.02
 C74-C76 \\sim C74-C75 \\sim C76-C75
 with sigma of 0.02
 O13A-O14A \\sim O13A-O15A \\sim O13A-O16A \\sim O14A-O15A \\sim O14A-O16A
\\sim O15A-O16A
 with sigma of 0.02
 Cl2-O13 \\sim Cl2-O14 \\sim Cl2-O15 \\sim Cl2-O16
 with sigma of 0.02
 O13-O14 \\sim O13-O15 \\sim O13-O16 \\sim O14-O15 \\sim O14-O16 \\sim O15-O16
 with sigma of 0.02
 Cl1-O9 \\sim Cl1-O10 \\sim Cl1-O11 \\sim Cl1-O12
 with sigma of 0.02
 O9-O10 \\sim O9-O11 \\sim O9-O12 \\sim O10-O11 \\sim O10-O12 \\sim O11-O12
 with sigma of 0.02
 N15-C95 \\sim N15-C94
 with sigma of 0.02
 N13-C89 \\sim N13-C88
 with sigma of 0.02
3. Restrained planarity
 O19, N15, C94, C95, C96
 with sigma of 0.1
 O17, N13, C88, C89, C90
 with sigma of 0.1
4. Rigid bond restraints
 C73, C74, C75, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2A, O13A, O14A, O15A, O16A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O13, O14, O15, O16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C73 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Cl2A \\sim O13A \\sim O14A \\sim O15A \\sim O16A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Cl2 \\sim O13 \\sim O14 \\sim O15 \\sim O16: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O19 \\sim N15 \\sim C94 \\sim C95 \\sim C96: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Cl1 \\sim O9 \\sim O10 \\sim O11 \\sim O12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O17 \\sim N13 \\sim C88 \\sim C89 \\sim C90: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
6. Rigid body (RIGU) restrains
 O19, N15, C94, C95, C96
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O9, O10, O11, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, N13, C88, C89, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(Cl2A)=Sof(O13A)=Sof(O14A)=Sof(O15A)=Sof(O16A)=1-FVAR(1)
 Sof(Cl2)=Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=FVAR(1)
8.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3), N4(H4), N6(H6), N7(H7), N9(H9), N10(H10), N12(H12)
8.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C22(H22A,H22B), C23(H23A,H23B),
  C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
 C52(H52A,H52B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
  C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C69(H69A,
 H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B)
8.c Me refined with everything fixed:
 C76(H76A,H76B,H76C), C87(H87A,H87B,H87C), C94(H94A,H94B,H94C), C95(H95A,H95B,
 H95C)
8.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C19(H19), C21(H21), C45(H45), C47(H47), C59(H59), C61(H61),
 C90(H90), C85(H85), C96(H96), C93(H93)
8.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C53(H53A,H53B,H53C),
 C68(H68A,H68B,H68C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C78(H78A,H78B,
 H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C84(H84A,
 H84B,H84C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C86(H86A,H86B,H86C),
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12959
_shelx_fab_checksum              37449
_olex2_submission_special_instructions 'No special instructions were received'