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_7123370
_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         '2(C58 H76 Mn2 O12 Sm2), 3(C4 H8 O)'
_chemical_formula_sum            'C128 H176 Mn4 O27 Sm4'
_chemical_formula_weight         2967.84
_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     dual
_audit_creation_date             2018-10-26
_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                101.808(3)
_cell_angle_beta                 94.242(3)
_cell_angle_gamma                90.676(3)
_cell_formula_units_Z            1
_cell_length_a                   12.6229(4)
_cell_length_b                   12.8766(4)
_cell_length_c                   20.6420(7)
_cell_measurement_reflns_used    24925
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      1.62
_cell_volume                     3273.91(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
 210 frames, detector distance = 100 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  0.0591
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34794
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.517
_diffrn_reflns_theta_min         1.616
_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    2.203
_exptl_absorpt_correction_T_max  0.6789
_exptl_absorpt_correction_T_min  0.5637
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       rod
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.499
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.069
_refine_diff_density_max         1.580
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         18120
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0552P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12194
_reflns_number_total             18120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02350j2.cif
_cod_data_source_block           ry347
_cod_database_code               7123370
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.406
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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
 C40-H50F
 2.4 with sigma of 0.02
 C59-C60 \\sim C60-C61 \\sim C61-C62
 with sigma of 0.02
 C60-C62 \\sim C59-C61
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O12 \\sim C55B \\sim C56 \\sim C57B \\sim C58B: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04
O12 \\sim C55A \\sim C56 \\sim C57A \\sim C58A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
C59 \\sim C60 \\sim C61 \\sim C62: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O13 \\sim C59 \\sim C60 \\sim C61 \\sim C62: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C59, C60, C61, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C45A(0.5) C46A(0.5) C47A(0.5) C48A(0.5) C49A(0.5) C50A(0.5)
 H50A(0.5) H50B(0.5) H50C(0.5) C51A(0.5) H51A(0.5) H51B(0.5) H51C(0.5)
 C52A(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53A(0.5) H53A(0.5) H53B(0.5)
 H53C(0.5) C54A(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C46B(0.5) C45B(0.5)
 C47B(0.5) C48B(0.5) C49B(0.5) C50B(0.5) H50D(0.5) H50E(0.5) H50F(0.5)
 C51B(0.5) H51D(0.5) H51E(0.5) H51F(0.5) C52B(0.5) H52D(0.5) H52E(0.5)
 H52F(0.5) C53B(0.5) H53D(0.5) H53E(0.5) H53F(0.5) C54B(0.5) H54D(0.5)
 H54E(0.5) H54F(0.5) C55A(0.5) H55A(0.5) H55B(0.5) C55B(0.5) H55C(0.5)
 H55D(0.5) H56A(0.5) H56B(0.5) H56C(0.5) H56D(0.5) C57A(0.5) H57A(0.5)
 H57B(0.5) C57B(0.5) H57C(0.5) H57D(0.5) C58A(0.5) H58A(0.5) H58B(0.5)
 C58B(0.5) H58C(0.5) H58D(0.5) O13(0.5) C59(0.5) H59A(0.5) H59B(0.5) C60(0.5)
 H60A(0.5) H60B(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5)
6.a :
 C45A(C46A,C47A,C48A,C49A,C50A,C51A,C52A,C53A,C54A), C46B(C45B,C47B,C48B,C49B,
 C50B,C51B,C52B,C53B,C54B)
6.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C55A(H55A,
 H55B), C55B(H55C,H55D), C56(H56A,H56B), C56(H56C,H56D), C57A(H57A,H57B),
 C57B(H57C,H57D), C58A(H58A,H58B), C58B(H58C,H58D), C63(H63A,H63B), C64(H64A,
 H64B), C65(H65A,H65B), C66(H66A,H66B), C59(H59A,H59B), C60(H60A,H60B),
 C61(H61A,H61B), C62(H62A,H62B)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C50A(H50A,H50B,H50C), C51A(H51A,H51B,H51C), C52A(H52A,H52B,H52C),
 C53A(H53A,H53B,H53C), C54A(H54A,H54B,H54C), C50B(H50D,H50E,H50F), C51B(H51D,
 H51E,H51F), C52B(H52D,H52E,H52F), C53B(H53D,H53E,H53F), C54B(H54D,H54E,H54F)
;
_shelx_res_checksum              34088
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'