Exploring Ligand Non-Innocence of Coordinatively-Versatile Diamidodipyrrinato Cobalt Complexes
Saund, Simran S.; Goldschmid, Samantha L.; Ng, Karina; Stewart, Veronica J.; Siegler, Maxime A.; Thoi, V. Sara; Chemical Communications  (2019) –; doi:10.1039/C8CC08674E

data_7122889
_publ_section_title
;
 Exploring Ligand Non-Innocence of Coordinatively-Versatile
 Diamidodipyrrinato Cobalt Complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08674E
_journal_year                    2019
_chemical_formula_moiety         'C46 H50 Co N8 O4, H2 O'
_chemical_formula_sum            'C46 H52 Co N8 O5'
_chemical_formula_weight         855.88
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-10-30 deposited with the CCDC.
2019-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9425(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.49785(11)
_cell_length_b                   23.1796(3)
_cell_length_c                   21.4226(3)
_cell_measurement_reflns_used    10781
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      72.03
_cell_measurement_theta_min      2.81
_cell_volume                     4645.49(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30176
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.893
_diffrn_reflns_theta_min         2.832
_exptl_absorpt_coefficient_mu    3.313
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
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            green
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         9073
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+2.4380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7929
_reflns_number_total             9073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08674e2.cif
_cod_data_source_block           2
_cod_original_cell_volume        4645.49(10)
_cod_database_code               7122889
_oxdiff_exptl_absorpt_empirical_full_min 0.693
_oxdiff_exptl_absorpt_empirical_full_max 1.470
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2014-3
_shelx_res_checksum              11675
_shelx_hkl_checksum              53616
_shelx_fab_checksum              11326