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_4348792
_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), 1.5(C H2 Cl2)'
_chemical_formula_sum            'C29.5 H75 B2 Cl3 F8 N4 P4 Re6 Se8'
_chemical_formula_weight         2638.66
_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'
_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                 92.5739(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2832(5)
_cell_length_b                   17.9598(8)
_cell_length_c                   27.4523(12)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.119
_cell_measurement_theta_min      2.386
_cell_volume                     6050.0(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            92970
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.355
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.061
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0896 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.6384.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.897
_exptl_crystal_description       block
_exptl_crystal_F_000             4780
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and diethyl ether by solvent layering'
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.087
_refine_diff_density_max         2.694
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         12371
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0207P)^2^+139.9752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10151
_reflns_number_total             12371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01643_si_004.cif
_cod_data_source_block           mo_cc30a_0m
_cod_original_formula_sum        'C29.50 H75 B2 Cl3 F8 N4 P4 Re6 Se8'
_cod_database_code               4348792
_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. Restrained distances
 N4-H4B = N4-H4A = N3-H3
 0.83 with sigma of 0.02
 N2-H2B = N2-H2A
 0.83 with sigma of 0.02
3. Rigid bond restraints
 C12, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C12, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C30(0.5) H30A(0.5) H30B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B),
 C21(H21A,H21B), C23(H23A,H23B), C29(H29A,H29B), C30(H30A,H30B)
7.b Idealised Me refined as rotating group:
 C2(H2C,H2D,H2E), C4(H4C,H4D,H4E), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              70033
_shelx_hkl_checksum              69665
_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 cc30a
_olex2_submission_special_instructions 'No special instructions were received'