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_7123367
_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         'C59 H78 Mn N4 O6 Sm, 1(C7 H8)'
_chemical_formula_sum            'C66 H86 Mn N4 O6 Sm'
_chemical_formula_weight         1236.67
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-16
_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                89.302(2)
_cell_angle_beta                 74.549(2)
_cell_angle_gamma                78.249(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3657(3)
_cell_length_b                   14.0273(3)
_cell_length_c                   19.3568(5)
_cell_measurement_reflns_used    33112
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.74
_cell_measurement_theta_min      1.79
_cell_volume                     3165.26(14)
_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 0.993
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
 254 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  0.0341
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31661
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.264
_diffrn_reflns_theta_min         1.793
_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    1.169
_exptl_absorpt_correction_T_max  0.9148
_exptl_absorpt_correction_T_min  0.7074
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       plate
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.271
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.805
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         16880
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13537
_reflns_number_total             16880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02350j2.cif
_cod_data_source_block           ry328y
_cod_database_code               7123367
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.652
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C45B \\sim C46B \\sim C47B: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C45A \\sim C46A \\sim C47A: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C47B) = Uanis(C47A)
Uanis(C45B) = Uanis(C45A)
3. Others
 Fixed Sof: C45B(0.4) H45B(0.4) C46B(0.4) H46A(0.4) H46B(0.4) H46C(0.4)
 C47B(0.4) H47A(0.4) H47B(0.4) H47C(0.4) C63A(0.66666) H63A(0.66666)
 C62A(0.66666) H62A(0.66666) C61A(0.66666) C66A(0.66666) H66A(0.66666)
 C65A(0.66666) H65A(0.66666) C64A(0.66666) H64A(0.66666) C45A(0.6) H45A(0.6)
 C46A(0.6) H46D(0.6) H46E(0.6) H46F(0.6) C47A(0.6) H47D(0.6) H47E(0.6)
 H47F(0.6) C60A(0.66666) H60A(0.66666) H60B(0.66666) H60C(0.66666) C60B(0.3333)
 H60D(0.3333) H60E(0.3333) H60F(0.3333) C63B(0.3333) H63B(0.3333) C62B(0.3333)
 H62B(0.3333) C61B(0.3333) C66B(0.3333) H66B(0.3333) C65B(0.3333) H65B(0.3333)
 C64B(0.3333) H64B(0.3333)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C20(H20), C23(H23), C33(H33), C36(H36), C45B(H45B),
 C48(H48), C45A(H45A)
4.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C16(H16), C17(H17), C18(H18), C29(H29), C30(H30),
 C31(H31), C41(H41), C42(H42), C43(H43), C63A(H63A), C62A(H62A), C66A(H66A),
 C65A(H65A), C64A(H64A), C63B(H63B), C62B(H62B), C66B(H66B), C65B(H65B),
 C64B(H64B)
4.d Fitted hexagon refined as free rotating group:
 C63A(C62A,C61A,C66A,C65A,C64A), C63B(C62B,C61B,C66B,C65B,C64B)
4.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C46B(H46A,H46B,H46C), C47B(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C46A(H46D,H46E,H46F), C47A(H47D,H47E,H47F),
 C60A(H60A,H60B,H60C), C60B(H60D,H60E,H60F)
;
_shelx_res_checksum              44617
_olex2_submission_special_instructions 'No special instructions were received'