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_7706490
_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 N4 Re Si, C5 H12'
_chemical_formula_sum            'C54 H81 N4 Re Si'
_chemical_formula_weight         1000.51
_chemical_melting_point          452(3)
_chemical_name_systematic        Re(Si[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
_audit_creation_date             2019-08-08
_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                96.261(2)
_cell_angle_beta                 92.718(2)
_cell_angle_gamma                102.594(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3802(3)
_cell_length_b                   12.9055(4)
_cell_length_c                   21.1791(5)
_cell_measurement_reflns_used    25641
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.7030
_cell_measurement_theta_min      3.2500
_cell_volume                     2480.54(13)
_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)'
_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 0.997
_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    -30.00  12.00   0.50    2.50    --   -1.86 -95.00 -40.00   84
  2  \w    -29.00  -4.00   0.50    2.50    --   -1.86  95.00  69.00   50
  3  \w     -3.00  23.00   0.50    2.50    --    2.17 -95.00 -40.00   52
  4  \w    -14.00  12.00   0.50    2.50    --    2.17  95.00  69.00   52
  5  \w    -17.00  28.00   0.50    2.50    --   -1.86  57.00 150.00   90
  6  \w     45.00  71.00   0.50    2.50    --   -1.86  57.00 150.00   52
  7  \w     -1.00  26.00   0.50    2.50    --   -1.86  77.00 150.00   54
  8  \w    -12.00  35.00   0.50    2.50    --    2.17 -99.00 -90.00   94
  9  \w     -2.00  74.00   0.50    2.50    --    2.17  57.00-150.00  152
 10  \w    -32.00  24.00   0.50    2.50    --    2.17 -77.00 -30.00  112
 11  \w    -28.00  24.00   0.50    2.50    --    2.17 -77.00-120.00  104
 12  \w    -12.00  36.00   0.50    2.50    --    2.17 -99.00 120.00   96
 13  \w    -72.00  14.00   0.50    2.50    --    2.17 -38.00-180.00  172
 14  \w    -11.00  34.00   0.50    2.50    --    2.17 -99.00-180.00   90
;
_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      -0.0382433000
_diffrn_orient_matrix_UB_12      -0.0151398000
_diffrn_orient_matrix_UB_13      -0.0304632000
_diffrn_orient_matrix_UB_21      0.0458620000
_diffrn_orient_matrix_UB_22      -0.0358069000
_diffrn_orient_matrix_UB_23      -0.0078741000
_diffrn_orient_matrix_UB_31      -0.0496991000
_diffrn_orient_matrix_UB_32      -0.0413335000
_diffrn_orient_matrix_UB_33      0.0122989000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50669
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.044
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.512
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35512
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.024
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         10121
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0401P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9051
_reflns_number_total             10121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00129a2.cif
_cod_data_source_block           1a_ReSi
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '449-454' was changed to
'452(3)' -- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7706490--7706495.cif.
;
_cod_database_code               7706490
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Re Si C30 H30 N2 '
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.661
_diffrn_oxdiff_digest_frames
;
01d167fedea7546f29a49ae3a1ddacad5001254b676
;
_diffrn_oxdiff_digest_hkl
;
019868c4d753257aaa0f259290af99417a8392
;
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C50-C51
 1.54 with sigma of 0.02
 C51-C52
 1.54 with sigma of 0.02
 C52-C53
 1.54 with sigma of 0.02
 C53-C54
 1.54 with sigma of 0.02
 C58-C59
 1.54 with sigma of 0.02
 C55-C56
 1.54 with sigma of 0.02
 C56-C57
 1.54 with sigma of 0.02
 C57-C58
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C52) = Uanis(C56)
4. Others
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C57)=
 Sof(H57A)=Sof(H57B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=
 Sof(H59C)=1-FVAR(1)
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=
 Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(H54C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C29(H29), C32(H32)
5.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C56(H56A,H56B), C57(H57A,
 H57B), C58(H58A,H58B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C13(H13), C14(H14), C15(H15),
 C25(H25), C26(H26), C27(H27), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
5.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              411
_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 4.635
_oxdiff_exptl_absorpt_empirical_full_min 0.245