Controlling dinitrogen functionalization at rhenium through alkali metal ion pairing.
Lohrey, Trevor D.; Bergman, Robert G.; Arnold, John; Dalton transactions (Cambridge, England : 2003) 48 (2019) 17936–17944; doi:10.1039/c9dt04489b

data_7703231
_publ_section_title
;
 Controlling dinitrogen functionalization at rhenium through alkali metal
 ion pairing.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17936
_journal_page_last               17944
_journal_paper_doi               10.1039/c9dt04489b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C43 H55 N3 Re, C24 H32 Na O8, 2(C4 H10 O)'
_chemical_formula_sum            'C75 H107 N3 Na O10 Re'
_chemical_formula_weight         1419.82
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-24 deposited with the CCDC.	2019-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                86.467(2)
_cell_angle_beta                 70.184(2)
_cell_angle_gamma                65.348(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4071(7)
_cell_length_b                   16.3244(8)
_cell_length_c                   17.5429(9)
_cell_measurement_reflns_used    50320
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.263
_cell_measurement_theta_min      2.373
_cell_volume                     3512.4(3)
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II CPAD detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50320
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.263
_diffrn_reflns_theta_min         2.373
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    1.900
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.275
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         14502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.5325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13367
_reflns_number_total             14502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04489b2.cif
_cod_data_source_block           shelx_CCDC4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7703231
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              23404