Cobalt-triphos dinitrogen complexes: activation and silyl-functionalisation of N2
Apps, Samantha; Miller, Philip; Long, Nicholas J.; Chemical Communications  (2019) –; doi:10.1039/C9CC01496A

data_7123425
_publ_section_title
;
 Cobalt-triphos dinitrogen complexes: activation and
 silyl-functionalisation of N2
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01496A
_journal_year                    2019
_chemical_formula_moiety         'C78 H72 Co2 N4 P6'
_chemical_formula_sum            'C78 H72 Co2 N4 P6'
_chemical_formula_weight         1369.07
_chemical_name_systematic        3
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.92580(10)
_cell_length_b                   18.92580(10)
_cell_length_c                   18.92580(10)
_cell_measurement_reflns_used    1876
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      72.5730
_cell_measurement_theta_min      4.6600
_cell_volume                     6778.95(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     52.00  94.00   1.00   10.95    --   41.86  19.00  30.00   42
  2  \w     26.00 104.00   1.00   41.73    --  106.38 -95.00 120.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0710501000
_diffrn_orient_matrix_UB_12      0.0159696000
_diffrn_orient_matrix_UB_13      -0.0364026000
_diffrn_orient_matrix_UB_21      0.0287992000
_diffrn_orient_matrix_UB_22      0.0305596000
_diffrn_orient_matrix_UB_23      0.0697057000
_diffrn_orient_matrix_UB_31      0.0272870000
_diffrn_orient_matrix_UB_32      -0.0737379000
_diffrn_orient_matrix_UB_33      0.0211105000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4814
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.488
_diffrn_reflns_theta_min         4.046
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       'irregular blocks'
_exptl_crystal_F_000             2848
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0551P)^2^+1.7943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1900
_reflns_number_total             2193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01496a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        6778.95(11)
_cod_database_code               7123425
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C39 H36 Co P3 N3'
_chemical_oxdiff_usercomment     SA272
_shelx_estimated_absorpt_t_max   0.507
_shelx_estimated_absorpt_t_min   0.335
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C15(H15), C11(H11), C8(H8), C6(H6), C5(H5), C9(H9), C12(H12),
 C14(H14), C13(H13)
;
_shelx_res_checksum              86024
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.076
_oxdiff_exptl_absorpt_empirical_full_min 0.972