σ or π? Bonding interactions in a series of rhenium metallotetrylenes.
Ouellette, Erik T.; Carpentier, Ambre; Joseph Brackbill, I.; Lohrey, Trevor D.; Douair, Iskander; Maron, Laurent; Bergman, Robert G.; Arnold, John; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2083–2092; doi:10.1039/d1dt00129a

data_7706492
_publ_section_title
;
 \s or \p? Bonding interactions in a series of rhenium metallotetrylenes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2083
_journal_page_last               2092
_journal_paper_doi               10.1039/d1dt00129a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C49 H69 Ge N4 Re'
_chemical_formula_sum            'C49 H69 Ge N4 Re'
_chemical_formula_weight         972.87
_chemical_name_systematic        Re(Ge[PhC(NtBu)2])(\h5-Cp)(BDI)
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-08 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                94.783(2)
_cell_angle_beta                 92.965(2)
_cell_angle_gamma                100.914(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3575(2)
_cell_length_b                   13.0104(3)
_cell_length_c                   20.9296(4)
_cell_measurement_reflns_used    20616
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.6670
_cell_measurement_theta_min      3.0840
_cell_volume                     2487.33(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  36.00   0.50    7.00    --   -1.86  83.00 103.00  126
  2  \w    -18.00   7.00   0.50    7.00    --    2.17  83.00 103.00   50
  3  \w     28.00  71.00   0.50    7.00    --   -1.86  57.00 -30.00   86
  4  \w     -1.00  82.00   0.50    7.00    --    2.17  19.00-180.00  166
  5  \w      3.00  28.00   0.50    7.00    --    2.17 -83.00 -16.00   50
  6  \w    -11.00  30.00   0.50    7.00    --    2.17 -99.00  60.00   82
  7  \w     -2.00  36.00   0.50    7.00    --    2.17 -99.00 120.00   76
  8  \w    -17.50  24.00   0.50    7.00    --   -1.86 -83.00 -16.00   83
  9  \w    -11.00  35.00   0.50    7.00    --    2.17 -99.00-120.00   92
 10  \w    -12.00  36.00   0.50    7.00    --    2.17 -99.00-150.00   96
 11  \w    -17.00  -6.00   0.50    7.00    --    2.17 -83.00 -16.00   22
 12  \w    -38.50 -17.00   0.50    7.00    --    2.17 -77.00  60.00   43
 13  \w    -74.00 -16.00   0.50    7.00    --   -1.86 -57.00-120.00  116
 14  \w    -17.00   9.00   0.50    7.00    --   -1.86  57.00 -30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0193767000
_diffrn_orient_matrix_UB_12      -0.0464424000
_diffrn_orient_matrix_UB_13      -0.0213720000
_diffrn_orient_matrix_UB_21      0.0531578000
_diffrn_orient_matrix_UB_22      0.0211872000
_diffrn_orient_matrix_UB_23      -0.0207846000
_diffrn_orient_matrix_UB_31      0.0527887000
_diffrn_orient_matrix_UB_32      -0.0224729000
_diffrn_orient_matrix_UB_33      0.0165327000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46677
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.859
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       prism
_exptl_crystal_F_000             996
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.607
_refine_diff_density_min         -1.541
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         10142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0412P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8838
_reflns_number_total             10142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00129a2.cif
_cod_data_source_block           2_ReGe
_cod_depositor_comments
'Adding full bibliography for 7706490--7706495.cif.'
_cod_database_code               7706492
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Re Si C45 H50 N4'
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.450
_diffrn_oxdiff_digest_frames
;
01faae9acb01498c879477bb519f5af9f80124200f4
;
_diffrn_oxdiff_digest_hkl
;
01290ab0179b6d55c04f99a00f7e8e1b8378b9
;
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C32(H32), C29(H29)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C4(H4), C1(H1), C5(H5), C3(H3), C27(H27), C26(H26), C37(H37),
 C25(H25), C15(H15), C41(H41), C13(H13), C39(H39), C38(H38), C40(H40), C14(H14)
2.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C48(H48A,H48B,
 H48C), C30(H30A,H30B,H30C), C21(H21A,H21B,H21C), C45(H45A,H45B,H45C), C19(H19A,
 H19B,H19C), C18(H18A,H18B,H18C), C49(H49A,H49B,H49C), C31(H31A,H31B,H31C),
 C34(H34A,H34B,H34C), C22(H22A,H22B,H22C), C44(H44A,H44B,H44C), C43(H43A,H43B,
 H43C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              53990
_shelx_fab_checksum              69257
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.837
_oxdiff_exptl_absorpt_empirical_full_min 0.216