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_7123423
_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         'C39 H36 Cl Co N P3'
_chemical_formula_sum            'C39 H36 Cl Co N P3'
_chemical_formula_weight         705.98
_chemical_name_systematic        1
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 99.940(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2110(4)
_cell_length_b                   20.2536(5)
_cell_length_c                   16.7695(5)
_cell_measurement_reflns_used    3594
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      27.8760
_cell_measurement_theta_min      2.9560
_cell_volume                     3416.03(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.819
_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     -2.00  82.00   1.00   18.79    --   14.27  57.00  90.00   84
  2  \w    -54.00  33.00   1.00   18.79    --   14.27 -37.00 -60.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0026876000
_diffrn_orient_matrix_UB_12      0.0283892000
_diffrn_orient_matrix_UB_13      0.0244089000
_diffrn_orient_matrix_UB_21      -0.0061988000
_diffrn_orient_matrix_UB_22      0.0202814000
_diffrn_orient_matrix_UB_23      -0.0349613000
_diffrn_orient_matrix_UB_31      -0.0701810000
_diffrn_orient_matrix_UB_32      -0.0028931000
_diffrn_orient_matrix_UB_33      -0.0053087000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12346
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.195
_diffrn_reflns_theta_min         2.402
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange/brown
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       'blocky needle'
_exptl_crystal_F_000             1464
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0479P)^2^+0.6123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5223
_reflns_number_total             6876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01496a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        3416.04(18)
_cod_database_code               7123423
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C39 H36 Cl Co N P3'
_chemical_oxdiff_usercomment     SA217
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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), C4(H4A,H4B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C19(H19), C35(H35), C33(H33), C21(H21), C22(H22), C12(H12), C9(H9),
 C31(H31), C30(H30), C16(H16), C42(H42), C37(H37), C15(H15), C10(H10), C17(H17),
  C23(H23), C18(H18), C29(H29), C11(H11), C39(H39), C25(H25), C28(H28),
 C13(H13), C27(H27), C36(H36), C41(H41), C24(H24), C34(H34), C40(H40)
;
_shelx_res_checksum              96777
_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 1.082
_oxdiff_exptl_absorpt_empirical_full_min 0.907