Tracking Pyrolysis Process of a 3-MeOsalophen-ligand based Co2 Complex for Promoted Oxygen Evolution Reaction
Pan, Bingxin; Peng, Xu; Wang, Yifan; An, Qi; Zhang, Xu; Zhang, Yuexing; Teets, Thomas S.; Zeng, Ming-Hua; Chemical Science  (2019) –; doi:10.1039/C9SC00505F

data_1550739
_publ_section_title
;
 Tracking Pyrolysis Process of a 3-MeOsalophen-ligand based Co2 Complex
 for Promoted Oxygen Evolution Reaction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00505F
_journal_year                    2019
_chemical_formula_moiety         'C23 H21 Cl3 Co2 N2 O6'
_chemical_formula_sum            'C23 H21 Cl3 Co2 N2 O6'
_chemical_formula_weight         645.63
_chemical_name_systematic        PBX
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-04 deposited with the CCDC.    2019-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.371(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9719(4)
_cell_length_b                   7.6746(3)
_cell_length_c                   24.3948(6)
_cell_measurement_reflns_used    6093
_cell_measurement_temperature    293
_cell_measurement_theta_max      75.6140
_cell_measurement_theta_min      2.9410
_cell_volume                     2802.24(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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    -64.00  24.00   0.50    0.66    --  -43.80  59.00  99.00  176
  2  \w    -42.00 -16.00   0.50    2.66    --  -90.25 125.00 120.00   52
  3  \w    -93.00 -68.00   0.50    2.66    --  -90.25 125.00 120.00   50
  4  \w   -102.00 -63.00   0.50    2.66    --  -90.25  59.00  99.00   78
  5  \w   -117.00 -22.00   0.50    0.66    --  -43.80 -59.00 -40.00  190
  6  \w   -132.00 -86.00   0.50    2.66    --  -90.25 -94.00  60.00   92
  7  \w   -158.00 -68.00   0.50    2.66    --  -90.25 -59.00 -40.00  180
  8  \w     62.00 101.00   0.50    0.66    --   43.80 178.00-120.00   78
  9  \w     98.00 136.00   0.50    2.66    --  111.75 125.00-150.00   76
 10  \w    141.00 177.00   0.50    2.66    --  111.75 125.00-150.00   72
 11  \w     89.00 178.00   0.50    2.66    --  111.75  61.00  30.00  178
 12  \w    147.00 175.00   0.50    2.66    --  111.75  59.00  99.00   56
 13  \w    119.00 144.00   0.50    2.66    --  111.75  59.00  99.00   50
 14  \w     92.00 170.00   0.50    2.66    --  111.75 125.00 -60.00  156
 15  \w     62.00 134.00   0.50    2.66    --  111.75 -59.00 -40.00  144
 16  \w     89.00 120.00   0.50    2.66    --  111.75-125.00-180.00   62
 17  \w     56.00 107.00   0.50    2.66    --  111.75 -94.00-120.00  102
 18  \w     38.00  67.00   0.50    2.66    --  111.75-125.00-180.00   58
 19  \w     39.00 110.00   0.50    2.66    --  111.75-125.00  30.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0741153000
_diffrn_orient_matrix_UB_12      -0.1249484000
_diffrn_orient_matrix_UB_13      0.0182930000
_diffrn_orient_matrix_UB_21      0.0629866000
_diffrn_orient_matrix_UB_22      -0.0726207000
_diffrn_orient_matrix_UB_23      0.0453411000
_diffrn_orient_matrix_UB_31      -0.0335529000
_diffrn_orient_matrix_UB_32      0.1394255000
_diffrn_orient_matrix_UB_33      0.0399978000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15871
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.064
_diffrn_reflns_theta_max         67.064
_diffrn_reflns_theta_min         2.952
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.243
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_preparation       'Solvothermal synthesis'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.760
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4922
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2390
_refine_ls_wR_factor_ref         0.2561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3806
_reflns_number_total             4922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00505f2.cif
_cod_data_source_block           1
_cod_database_code               1550739
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H N O Co Cl'
_reflns_odcompleteness_completeness 98.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C24, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C24 \\sim O5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C24) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: C23(0.5) H23a(0.5) H23b(0.5) H23c(0.5) C24(0.5) H24a(0.5)
 H24b(0.5) H24c(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C17(H17), C18(H18), C19(H19)
5.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c)
;
_shelx_res_checksum              82610
_shelx_fab_checksum              59906
_olex2_submission_original_sample_id PBX
_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 2.182
_oxdiff_exptl_absorpt_empirical_full_min 0.420