N-H cleavage as a route to new pincer complexes of high-valent rhenium.
Kosanovich, Alex J.; Shih, Wei-Chun; Ramírez-Contreras, Rodrigo; Ozerov, Oleg V.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18532–18540; doi:10.1039/c6dt03640f

data_7040927
_publ_section_title
;
 N-H cleavage as a route to new pincer complexes of high-valent rhenium.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18532
_journal_page_last               18540
_journal_paper_doi               10.1039/c6dt03640f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C26 H40 Cl2 N O P2 Re'
_chemical_formula_sum            'C26 H40 Cl2 N O P2 Re'
_chemical_formula_weight         701.63
_chemical_name_systematic        '(PNP)ReOCl2 '
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_audit_update_record
;
2016-09-16 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.623(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.161(4)
_cell_length_b                   9.687(3)
_cell_length_c                   12.882(4)
_cell_measurement_reflns_used    8699
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.453
_cell_measurement_theta_min      2.221
_cell_volume                     1368.9(8)
_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, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15490
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.771
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1282 before and 0.0384 after correction.
The Ratio of minimum to maximum transmission is 0.6009.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       plate
_exptl_crystal_F_000             700
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CDCl3'
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.340
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0045P)^2^+3.9674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3007
_reflns_number_total             3129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03640f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7040927--7040930.cif.'
_cod_database_code               7040927
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.284
_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. Others
 Fixed Sof: Re1(0.5) Cl1(0.5) O1(0.5)
3.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              75042
_olex2_submission_special_instructions 'No special instructions were received'