High-valent nitridorhenium(v) complexes containing PNP ligands: implications of ligand flexibility.
Lambic, Nikola S.; Sommer, Roger D.; Ison, Elon A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 758–768; doi:10.1039/c7dt03615a

data_7044989
_publ_section_title
;
 High-valent nitridorhenium(v) complexes containing PNP ligands:
 implications of ligand flexibility.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              758
_journal_page_last               768
_journal_paper_doi               10.1039/c7dt03615a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C36 H52 N3 P2 Re'
_chemical_formula_sum            'C36 H52 N3 P2 Re'
_chemical_formula_weight         774.94
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-05-03 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7663(5)
_cell_length_b                   14.1650(4)
_cell_length_c                   35.8694(12)
_cell_measurement_reflns_used    7832
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.27
_cell_volume                     6994.5(4)
_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      101.6
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37210
_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         28.772
_diffrn_reflns_theta_min         2.140
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.594
_exptl_absorpt_correction_T_max  0.7201
_exptl_absorpt_correction_T_min  0.6060
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0499 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.8415.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.409
_refine_diff_density_min         -2.690
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         9080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+17.4734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7396
_reflns_number_total             9080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03615a3.cif
_cod_data_source_block           rds539_0m
_cod_depositor_comments
'Adding full bibliography for 7044989--7044991.cif.'
_cod_database_code               7044989
_publcif_datablock.id            {a23fdc6c-1130-47ef-9784-b6f24de40edc}
_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:
 C1(H1), C4(H4), C21(H21), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C13(H13), C15(H15), C16(H16), C19(H19), C31(H31), C32(H32),
 C33(H33)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C12(H12A,
 H12B,H12C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              72962
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'