Syntheses, Rearrangements, and Structural Analyses of Unsaturated Nitrogen Donor Ligands Derived from Diphenyldiazomethane and the Chiral Rhenium Lewis Acid [(η5-C5H5)Re(NO)(PPh3)]+
Estrada, Alexander Louis; Wititsuwannakul, Taveechai; Kromm, Klemenz; Hampel, Frank; Hall, Michael B.; Gladysz, John; Dalton Transactions  (2022) –; doi:10.1039/D2DT00890D

data_7710073
_publ_section_title
;
 Syntheses, Rearrangements, and Structural Analyses of Unsaturated
 Nitrogen Donor Ligands Derived from Diphenyldiazomethane and the Chiral
 Rhenium Lewis Acid [(\h5-C5H5)Re(NO)(PPh3)]+
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00890D
_journal_year                    2022
_chemical_formula_moiety         'C36 H29 N3 O P Re, C H2 Cl2'
_chemical_formula_sum            'C37 H31 Cl2 N3 O P Re'
_chemical_formula_weight         821.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-10-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2022-03-16 deposited with the CCDC.	2022-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.4775(2)
_cell_length_b                   18.2342(5)
_cell_length_c                   34.1669(7)
_cell_measurement_reflns_used    5729
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     6527.5(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            10292
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.234
_exptl_absorpt_coefficient_mu    3.971
_exptl_absorpt_correction_T_max  0.6922
_exptl_absorpt_correction_T_min  0.5039
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Scalepack
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3248
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and hexane  by solvent layering'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0239P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3439
_reflns_number_total             5709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00890d3.cif
_cod_data_source_block           klk12
_cod_database_code               7710073
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.504
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All Cl(H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,
  H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C13) = Uanis(C15) = Uanis(C11)
Uanis(C12) = Uanis(C11) = Uanis(C15) = Uanis(C14) = Uanis(C13)
3.a Riding coordinates:
 Cl11(H11,H12,H13,H14,H15,H22,H23,H24,H25,H26,H32,H33,H34,H35,H36,H42,H43,H44,
 H45,H46,H52,H53,H54,H55,H56,H63,H64,H65,H66)
3.b Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B)
;
_shelx_res_checksum              63958
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre in perfluoroether oil'
_olex2_submission_original_sample_id 'KK III / 10'
_olex2_submission_special_instructions 'No special instructions were received'