Heterotetrametallic Re-Zn-Zn-Re Complex Generated by an Anionic Rhenium(I) β-Diketiminate.
Lohrey, Trevor D.; Maron, Laurent; Bergman, Robert G.; Arnold, John; Journal of the American Chemical Society 141 (2019) 800–804; doi:10.1021/jacs.8b12494

data_4133653
_publ_section_title
;
 Heterotetrametallic Re-Zn-Zn-Re Complex Generated by an Anionic
 Rhenium(I) \b-Diketiminate.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              800
_journal_page_last               804
_journal_paper_doi               10.1021/jacs.8b12494
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.5(C68 H92 N4 Na2 Re2)'
_chemical_formula_sum            'C34 H46 N2 Na Re'
_chemical_formula_weight         691.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-13
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1625(3)
_cell_length_b                   21.0519(7)
_cell_length_c                   12.4534(4)
_cell_measurement_reflns_used    14047
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5820
_cell_measurement_theta_min      3.3090
_cell_volume                     3188.62(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -25.00   1.00   0.50    2.73    --   -1.86  77.00-120.00   52
  2  \w     -3.00  31.00   0.50    2.73    --   -1.86 -99.00 -30.00   68
  3  \w    -41.00  24.00   0.50    2.73    --    2.17 -77.00  60.00  130
  4  \w    -15.00  41.00   0.50    2.73    --    2.17  77.00 -60.00  112
  5  \w     -2.00  38.00   0.50    2.73    --    2.17  38.00 -90.00   80
  6  \w     49.00  78.00   0.50    2.73    --    2.17  38.00 -90.00   58
  7  \w    -32.00  12.00   0.50    2.73    --    2.17 -19.00 -60.00   88
  8  \w    -45.00 -19.00   0.50    2.73    --    2.17 -77.00   0.00   52
  9  \w    -68.00 -39.00   0.50    2.73    --    2.17 -19.00 -60.00   58
 10  \w    -12.00  30.00   0.50    2.73    --    2.17  77.00-180.00   84
;
_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      0.0169624000
_diffrn_orient_matrix_UB_12      -0.0286926000
_diffrn_orient_matrix_UB_13      0.0248363000
_diffrn_orient_matrix_UB_21      0.0002205000
_diffrn_orient_matrix_UB_22      -0.0153517000
_diffrn_orient_matrix_UB_23      -0.0507289000
_diffrn_orient_matrix_UB_31      0.0557841000
_diffrn_orient_matrix_UB_32      0.0087589000
_diffrn_orient_matrix_UB_33      -0.0073346000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1316
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.332
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45f (Rigaku Oxford Diffraction, 2018)
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    1.441
_exptl_crystal_description       plank
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.307
_refine_diff_density_min         -1.997
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0571P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2898
_reflns_number_total             3350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12494_si_002.cif
_cod_data_source_block           tl6181
_cod_original_cell_volume        3188.61(17)
_cod_database_code               4133653
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Na Re C H N'
_reflns_odcompleteness_completeness 99.65
_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:
 C7(H7), C18(H18), C14(H14)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C),
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              39431
_shelx_hkl_checksum              20784
_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 3.147
_oxdiff_exptl_absorpt_empirical_full_min 0.336