Rhenium is different: CO tetramerization induced by a divalent lanthanide complex in rhenium carbonyls
Yadav, Ravi; Simler, Thomas; Gamer, Michael T.; Köppe, Ralf; Roesky, Peter W.; Chemical Communications  (2019) –; doi:10.1039/C9CC02350J

data_7123366
_publ_section_title
;
 Rhenium is different: CO tetramerization induced by a divalent lanthanide
 complex in rhenium carbonyls
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02350J
_journal_year                    2019
_chemical_formula_moiety         'C96 H128 O13 Re2 Sm4, 4(C7 H8)'
_chemical_formula_sum            'C124 H160 O13 Re2 Sm4'
_chemical_formula_weight         2832.31
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-22 deposited with the CCDC.    2019-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.4540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1910(3)
_cell_length_b                   26.5776(7)
_cell_length_c                   28.8827(6)
_cell_measurement_reflns_used    104021
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      1.32
_cell_volume                     11979.4(5)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
 273 frames, detector distance = 135 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            73301
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.603
_diffrn_reflns_theta_min         1.315
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.998
_exptl_absorpt_correction_T_max  0.9379
_exptl_absorpt_correction_T_min  0.7197
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       prism
_exptl_crystal_F_000             5624
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.076
_refine_diff_density_max         3.319
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.177
_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     1205
_refine_ls_number_reflns         22410
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+58.4517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18613
_reflns_number_total             22410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02350j2.cif
_cod_data_source_block           ry360
_cod_database_code               7123366
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.316
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C104-C105
 1.47 with sigma of 0.02
 C110-C104 \\sim C104-C106
 with sigma of 0.02
 C96-C95A \\sim C95A-C94
 with sigma of 0.02
 C103-C97 \\sim C97-C99
 with sigma of 0.02
 C205-C206 \\sim C206-C207 \\sim C207-C208 \\sim C208-C209 \\sim C209-C210
\\sim C210-C205
 with sigma of 0.02
 C205-C209 \\sim C205-C207 \\sim C210-C208 \\sim C206-C210 \\sim C207-C209
\\sim C206-C208
 with sigma of 0.04
 C204-C210 \\sim C204-C206
 with sigma of 0.04
 C298-C299 \\sim C299-C200 \\sim C200-C201 \\sim C201-C202 \\sim C202-C203
\\sim C203-C298
 with sigma of 0.02
 C298-C202 \\sim C298-C200 \\sim C203-C201 \\sim C299-C203 \\sim C200-C202
\\sim C299-C201
 with sigma of 0.04
 C297-C203 \\sim C297-C299
 with sigma of 0.04
 C119-C120 \\sim C120-C121 \\sim C121-C122 \\sim C122-C123 \\sim C123-C124
\\sim C124-C119
 with sigma of 0.02
 C119-C123 \\sim C119-C121 \\sim C124-C122 \\sim C120-C124 \\sim C121-C123
\\sim C120-C122
 with sigma of 0.04
 C118-C124 \\sim C118-C120
 with sigma of 0.04
 C219-C220 \\sim C220-C221 \\sim C221-C222 \\sim C222-C223 \\sim C223-C224
\\sim C224-C219
 with sigma of 0.02
 C219-C223 \\sim C219-C221 \\sim C224-C222 \\sim C220-C224 \\sim C221-C223
\\sim C220-C222
 with sigma of 0.04
 C218-C224 \\sim C218-C220
 with sigma of 0.04
 C112-C117 \\sim C117-C116 \\sim C116-C115 \\sim C115-C114 \\sim C114-C113
\\sim C113-C112
 with sigma of 0.02
 C112-C114 \\sim C112-C116 \\sim C113-C115 \\sim C117-C113 \\sim C116-C114
\\sim C117-C115
 with sigma of 0.04
 C111-C113 \\sim C111-C117
 with sigma of 0.04
3. Restrained planarity
 C204, C205, C206, C207, C208, C209, C210
 with sigma of 0.1
 C298, C200, C201, C202, C203, C297, C299
 with sigma of 0.1
 C118, C119, C120, C121, C122, C123, C124
 with sigma of 0.1
 C218, C222, C220, C224, C219, C221, C223
 with sigma of 0.1
 C111, C112, C113, C114, C115, C116, C117
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C93 \\sim C94 \\sim C96 \\sim C95B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C93 \\sim C94 \\sim C95A \\sim C96: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C94 \\sim C96 \\sim C95B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04
C104 \\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C214 \\sim C212 \\sim C216 \\sim C211 \\sim C213 \\sim C215 \\sim C217: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C204 \\sim C205 \\sim C206 \\sim C207 \\sim C208 \\sim C209 \\sim C210: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C297 \\sim C298 \\sim C299 \\sim C200 \\sim C201 \\sim C202 \\sim C203: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C218 \\sim C222 \\sim C220 \\sim C224 \\sim C219 \\sim C221 \\sim C223: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C204, C205, C206, C207, C208, C209, C210
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C297, C298, C299, C200, C201, C202, C203
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C118, C119, C120, C121, C122, C123, C124
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C218, C222, C220, C224, C219, C221, C223
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C111, C112, C113, C114, C115, C116, C117
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H94C(0.33333) H94D(0.33333) H94A(0.66667) H94B(0.66667)
 C95A(0.66667) H95A(0.66667) H95B(0.66667) H96C(0.33333) H96D(0.33333)
 H96A(0.66667) H96B(0.66667) C218(0.5) H21D(0.5) H21E(0.5) H21F(0.5) C222(0.5)
 H222(0.5) C220(0.5) H220(0.5) C224(0.5) H224(0.5) C219(0.5) C221(0.5)
 H221(0.5) C223(0.5) H223(0.5) C95B(0.33333) H95C(0.33333) H95D(0.33333)
 C97(0.66667) H97A(0.66667) H97B(0.66667) H97C(0.66667) C98(0.66667)
 C103(0.66667) H103(0.66667) C102(0.66667) H102(0.66667) C101(0.66667)
 H101(0.66667) C100(0.66667) H100(0.66667) C99(0.66667) H99(0.66667)
 C104(0.66667) H10A(0.66667) H10B(0.66667) H10C(0.66667) C105(0.66667)
 C110(0.66667) H110(0.66667) C109(0.66667) H109(0.66667) C108(0.66667)
 H108(0.66667) C107(0.66667) H107(0.66667) C106(0.66667) H106(0.66667)
 C212(0.5) C213(0.5) H213(0.5) C214(0.5) H214(0.5) C215(0.5) H215(0.5)
 C216(0.5) H216(0.5) C217(0.5) H217(0.5) C111(0.5) H11A(0.5) H11B(0.5)
 H11C(0.5) C112(0.5) C113(0.5) H113(0.5) C114(0.5) H114(0.5) C115(0.5)
 H115(0.5) C116(0.5) H116(0.5) C117(0.5) H117(0.5) C118(0.5) H11D(0.5)
 H11E(0.5) H11F(0.5) C119(0.5) C120(0.5) H120(0.5) C121(0.5) H121(0.5)
 C122(0.5) H122(0.5) C123(0.5) H123(0.5) C124(0.5) H124(0.5) C211(0.5)
 H21G(0.5) H21H(0.5) H21I(0.5) C204(0.33333) H20D(0.33333) H20E(0.33333)
 H20F(0.33333) C205(0.33333) C206(0.33333) H206(0.33333) C207(0.33333)
 H207(0.33333) C208(0.33333) H208(0.33333) C209(0.33333) H209(0.33333)
 C210(0.33333) H210(0.33333) C297(0.3333) H29D(0.3333) H29E(0.3333)
 H29F(0.3333) C298(0.3333) C200(0.3333) H200(0.3333) C201(0.3333) H201(0.3333)
 C202(0.3333) H202(0.3333) C203(0.3333) H203(0.3333) C299(0.3333) H299(0.3333)
7.a Free rotating group:
 C218(C222,C220,C224,C219,C221,C223), C111(C112,C113,C114,C115,C116,C117),
 C118(C119,C120,C121,C122,C123,C124), C204(C205,C206,C207,C208,C209,C210),
 C297(C298,C200,C201,C202,C203,C299)
7.b Secondary CH2 refined with riding coordinates:
 C93(H93A,H93B), C94(H94C,H94D), C94(H94A,H94B), C95A(H95A,H95B), C96(H96C,
 H96D), C96(H96A,H96B), C95B(H95C,H95D)
7.c Me refined with riding coordinates:
 C70(H70A,H70B,H70C)
7.d Aromatic/amide H refined with riding coordinates:
 C222(H222), C220(H220), C224(H224), C221(H221), C223(H223), C103(H103),
 C102(H102), C101(H101), C100(H100), C99(H99), C110(H110), C109(H109),
 C108(H108), C107(H107), C106(H106), C213(H213), C214(H214), C215(H215),
 C216(H216), C217(H217), C113(H113), C114(H114), C115(H115), C116(H116),
 C117(H117), C120(H120), C121(H121), C122(H122), C123(H123), C124(H124),
 C206(H206), C207(H207), C208(H208), C209(H209), C210(H210), C200(H200),
 C201(H201), C202(H202), C203(H203), C299(H299)
7.e Fitted hexagon refined as free rotating group:
 C98(C103,C102,C101,C100,C99), C105(C110,C109,C108,C107,C106), C212(C213,C214,
 C215,C216,C217)
7.f Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C78(H78A,
 H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C),
 C82(H82A,H82B,H82C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,
 H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C218(H21D,H21E,H21F),
 C97(H97A,H97B,H97C), C104(H10A,H10B,H10C), C111(H11A,H11B,H11C), C118(H11D,
 H11E,H11F), C211(H21G,H21H,H21I), C204(H20D,H20E,H20F), C297(H29D,H29E,H29F)
;
_shelx_res_checksum              25196
_olex2_submission_special_instructions 'No special instructions were received'