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_7123369
_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 Yb, 1.5(C7 H8)'
_chemical_formula_sum            'C69.5 H90 Mn N4 O6 Yb'
_chemical_formula_weight         1305.43
_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             2018-10-17
_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                90.345(4)
_cell_angle_beta                 96.876(4)
_cell_angle_gamma                98.184(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1458(6)
_cell_length_b                   13.5433(7)
_cell_length_c                   19.7641(10)
_cell_measurement_reflns_used    44823
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.09
_cell_measurement_theta_min      2.12
_cell_volume                     3193.9(3)
_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      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.766
_diffrn_measurement_details
;
 396 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.766
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30724
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.766
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.064
_diffrn_reflns_theta_min         2.431
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.706
_exptl_absorpt_correction_T_max  0.7621
_exptl_absorpt_correction_T_min  0.5320
_exptl_absorpt_correction_type   multi-scan
_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.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         15702
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0365P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13513
_reflns_number_total             15702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02350j2.cif
_cod_data_source_block           ry330
_cod_original_formula_sum        'C69.50 H90 Mn N4 O6 Yb'
_cod_database_code               7123369
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.634
_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. Restrained distances
 C68-C73 \\sim C73-C72 \\sim C72-C71 \\sim C71-C70 \\sim C70-C69 \\sim C69-C68
 with sigma of 0.02
 C68-C70 \\sim C68-C72 \\sim C69-C71 \\sim C73-C69 \\sim C72-C70 \\sim C73-C71
 with sigma of 0.04
 C67-C69 \\sim C67-C73
 with sigma of 0.04
3. Restrained planarity
 C67, C68, C69, C70, C71, C72, C73
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C67, C68, C69, C70, C71, C72, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C68(0.5) C69(0.5) H69(0.5)
 C70(0.5) H70(0.5) C71(0.5) H71(0.5) C72(0.5) H72(0.5) C73(0.5) H73(0.5)
7.a Free rotating group:
 C67(C68,C69,C70,C71,C72,C73)
7.b Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C20(H20), C23(H23), C33(H33), C36(H36), C45(H45), C48(H48)
7.c Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B)
7.d 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), C69(H69), C70(H70), C71(H71), C72(H72),
  C73(H73), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
7.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), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C67(H67A,H67B,H67C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              11171
_olex2_submission_special_instructions 'No special instructions were received'