Ligand dechelation effect on a [Co(tpy)2]2+ scaffold towards electro-catalytic proton and water reduction
Majee, Karunamay; Padhi, Sumanta Kumar; New Journal of Chemistry 43 (2019) 3856–; doi:10.1039/C8NJ05712E

data_7058142
_publ_section_title
;
 Ligand dechelation effect on a [Co(tpy)2]2+ scaffold towards
 electro-catalytic proton and water reduction
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3856
_journal_paper_doi               10.1039/C8NJ05712E
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C48 H31 Co N8, 2(Cl), 3.5(H2 O)'
_chemical_formula_sum            'C48 H38 Cl2 Co N8 O3.5'
_chemical_formula_weight         912.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-08-23 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                94.018(3)
_cell_angle_beta                 100.907(4)
_cell_angle_gamma                100.487(4)
_cell_formula_units_Z            2
_cell_length_a                   8.9073(6)
_cell_length_b                   12.9124(4)
_cell_length_c                   21.2304(6)
_cell_measurement_reflns_used    5297
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.9960
_cell_measurement_theta_min      3.6440
_cell_volume                     2343.79(19)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0606
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       \w-scans
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0037
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10544
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'brownish red'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0017(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         10544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1063P)^2^+1.6832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2006
_reflns_number_gt                10487
_reflns_number_total             10544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj05712e2.cif
_cod_data_source_block           km
_cod_depositor_comments
;
         Adding full bibliography for 7058142.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H76 Cl4 Co2 N16 O7'
_cod_original_formula_weight         1825.39
_cod_original_formula_moiety         '2(C48 H31 Co N8), 4(Cl), 6(H2 O), O'
_cod_original_formula_units_Z            1
_cod_database_code               7058142
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Free rotating group:
 O3(H3A,H3B), O1(H1A,H1B), O2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C21(H21), C44(H44), C30(H30), C14(H14), C36(H36), C25(H25), C22(H22),
 C1(H1), C23(H23), C3(H3), C40(H40), C4(H4), C35(H35), C26(H26), C37(H37),
 C20(H20), C41(H41), C46(H46), C12(H12), C38(H38), C2(H2), C24(H24), C43(H43),
 C45(H45), C13(H13), C32(H32), C18(H18), C27(H27), C15(H15), C17(H17)
;
_olex2_submission_original_sample_id Co4ql-tpy
_olex2_submission_special_instructions 'No special instructions were received'