Synthesis and Thermal Properties of Novel NHC-Stabilized Cobalt Carbonyl Nitrosyl Complexes
Hering, Florian; Berthel, Johannes H. J.; Lubitz, Katharina; Paul, Ursula S. D.; Schneider, Heidi; Härterich, Marcel; Radius, Udo; Organometallics 35 (2016) 2806–; doi:10.1021/acs.organomet.6b00374

data_4088744
_publ_section_title
;
 Synthesis and Thermal Properties of Novel NHC-Stabilized Cobalt Carbonyl
 Nitrosyl Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2806
_journal_paper_doi               10.1021/acs.organomet.6b00374
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C13 H20 Co N3 O3'
_chemical_formula_weight         325.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0481(14)
_cell_length_b                   9.5636(9)
_cell_length_c                   10.3892(9)
_cell_measurement_reflns_used    5825
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.33
_cell_volume                     1594.5(2)
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_collection       'APEX2 ver. 2014.1 (Bruker AXS)'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_molecular_graphics    'XP in ShelxTL-97'
_computing_publication_material  'XP in ShelxTL-97'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20214
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.987
_diffrn_reflns_theta_min         2.335
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Sadabs 2012/1 (Bruker 2012)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       needle
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0865P)^2^+3.6312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1313
_reflns_number_total             1662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00374_si_002.cif
_cod_data_source_block           compound_10
_cod_database_code               4088744
_shelx_estimated_absorpt_t_min   0.702
_shelx_estimated_absorpt_t_max   0.928
_shelxl_version_number           2013-4
_shelx_res_checksum              3088
_shelx_hkl_checksum              90881