Amidine Production by the Addition of NH<sub>3</sub> to Nitrile(s) Bound to and Activated by the Lewis Acidic [Re<sub>6</sub>(μ<sub>3</sub>-Se)<sub>8</sub>]<sup>2+</sup> Cluster Core.
Corbin, William C.; Nichol, Gary S.; Zheng, Zhiping; Inorganic chemistry 55 (2016) 9505–9508; doi:10.1021/acs.inorgchem.6b01643

data_4348793
_publ_section_title
;
 Amidine Production by the Addition of NH<sub>3</sub> to Nitrile(s) Bound
 to and Activated by the Lewis Acidic
 [Re<sub>6</sub>(\m<sub>3</sub>-Se)<sub>8</sub>]<sup>2+</sup> Cluster
 Core.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9505
_journal_page_last               9508
_journal_paper_doi               10.1021/acs.inorgchem.6b01643
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C28 H72 N4 P4 Re6 Se8, 2(B F4)'
_chemical_formula_sum            'C28 H72 B2 F8 N4 P4 Re6 Se8'
_chemical_formula_weight         2511.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.037(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7462(8)
_cell_length_b                   20.1379(16)
_cell_length_c                   12.7725(8)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.319
_cell_measurement_theta_min      2.566
_cell_volume                     2748.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            38390
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         1.906
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.626
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0689 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.7851.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.034
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and diethyl ether by solvent layering'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.000126(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0231
_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^)+22.3051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4902
_reflns_number_total             5421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01643_si_003.cif
_cod_data_source_block           mo_cc31b_0m
_cod_database_code               4348793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{F1, F1'}
3. Restrained distances
 N2-H2
 0.86 with sigma of 0.02
 N3-H3A = N3-H3B = N2-H2
 0.83 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F1')
5. Rigid body (RIGU) restrains
 F2', F3', F4', B1'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{F1, F2, F3, F4, B1} sigma for 1-2: 0.02, 1-3: 0.02
as
{F1', F2', F3', F4', B1'}
7. Others
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(F4')=Sof(B1')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(B1)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3C,H3D), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B)
8.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              39012
_shelx_hkl_checksum              69675
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in Paratone oil'
_olex2_submission_original_sample_id CC31b
_olex2_submission_special_instructions 'No special instructions were received'