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_7123368
_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         'C58 H78 N4 O5 Re Sm, C7 H8'
_chemical_formula_sum            'C65 H86 N4 O5 Re Sm'
_chemical_formula_weight         1339.92
_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             2018-10-18
_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                 96.237(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7981(4)
_cell_length_b                   19.3819(5)
_cell_length_c                   19.0314(6)
_cell_measurement_reflns_used    30543
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      1.50
_cell_volume                     6159.6(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      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 0.991
_diffrn_measurement_details
;
 106 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  0.0382
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32481
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.544
_diffrn_reflns_theta_min         1.504
_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    2.957
_exptl_absorpt_correction_T_max  0.7845
_exptl_absorpt_correction_T_min  0.5433
_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    1.445
_exptl_crystal_description       prism
_exptl_crystal_F_000             2724
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.166
_refine_diff_density_max         1.769
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         17078
_refine_ls_number_restraints     206
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0497P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12990
_reflns_number_total             17078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02350j2.cif
_cod_data_source_block           ry339
_cod_original_cell_volume        6159.5(3)
_cod_database_code               7123368
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.378
_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
 C60B-C61B \\sim C61B-C62B \\sim C62B-C63B \\sim C63B-C64B \\sim C64B-C65B
\\sim C65B-C60B
 with sigma of 0.02
 C60B-C64B \\sim C60B-C62B \\sim C65B-C63B \\sim C61B-C65B \\sim C62B-C64B
\\sim C61B-C63B
 with sigma of 0.04
 C59B-C65B \\sim C59B-C61B
 with sigma of 0.04
 C64A-C63A \\sim C63A-C62A \\sim C62A-C61A \\sim C61A-C60A
 with sigma of 0.02
 C60A-C62A \\sim C60A-C64A \\sim C61A-C63A \\sim C64A-C62A
 with sigma of 0.04
3. Restrained planarity
 C59B, C60B, C61B, C62B, C63B, C64B, C65B
 with sigma of 0.1
 C59A, C60A, C61A, C62A, C63A, C64A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C59B \\sim C60B \\sim C61B \\sim C62B \\sim C63B \\sim C64B \\sim C65B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C59A \\sim C60A \\sim C61A \\sim C62A \\sim C63A \\sim C64A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C59A \\sim C60A \\sim C61A \\sim C62A \\sim C63A \\sim C64A \\sim C65A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C59B, C60B, C61B, C62B, C63B, C64B, C65B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C59A, C60A, C61A, C62A, C63A, C64A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C59A(0.5) H59A(0.5) H59B(0.5) H59C(0.5) C60A(0.5) C61A(0.5)
 H61A(0.5) C62A(0.5) H62A(0.5) C63A(0.5) H63A(0.5) C64A(0.5) H64A(0.5)
 C65A(0.5) H65A(0.5) C59B(0.5) H59D(0.5) H59E(0.5) H59F(0.5) C60B(0.5)
 C61B(0.5) H61B(0.5) C62B(0.5) H62B(0.5) C63B(0.5) H63B(0.5) C64B(0.5)
 H64B(0.5) C65B(0.5) H65B(0.5)
7.a Free rotating group:
 C59A(C60A,C61A,C62A,C63A,C64A), C59B(C60B,C61B,C62B,C63B,C64B,C65B)
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:
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C16(H16), C17(H17), C18(H18), C26(H26),
 C29(H29), C30(H30), C31(H31), C41(H41), C42(H42), C43(H43), C61A(H61A),
 C62A(H62A), C63A(H63A), C64A(H64A), C65A(H65A), C61B(H61B), C62B(H62B),
 C63B(H63B), C64B(H64B), C65B(H65B)
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), C59A(H59A,H59B,H59C), C59B(H59D,H59E,H59F)
;
_shelx_res_checksum              88592
_olex2_submission_special_instructions 'No special instructions were received'