Positional effects of second-sphere amide pendants on electrochemical CO<sub>2</sub> reduction catalyzed by iron porphyrins.
Nichols, Eva M.; Derrick, Jeffrey S.; Nistanaki, Sepand K.; Smith, Peter T.; Chang, Christopher J.; Chemical science 9 (2018) 2952–2960; doi:10.1039/c7sc04682k

data_1548976
_publ_section_title
;
 Positional effects of second-sphere amide pendants on electrochemical
 CO<sub>2</sub> reduction catalyzed by iron porphyrins.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              2952
_journal_page_last               2960
_journal_paper_doi               10.1039/c7sc04682k
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C58.5 H43.5 F6 N6.5 O2.5 Zn'
_chemical_formula_weight         1056.87
_chemical_name_systematic        Zn-ortho-1-amide
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-01-29 deposited with the CCDC.
2018-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.394(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.7604(6)
_cell_length_b                   51.619(2)
_cell_length_c                   18.6745(9)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.50
_cell_measurement_theta_min      2.21
_cell_volume                     10261.5(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL MULTI-CPU VERSION'
_computing_structure_solution    'SHELXT 2014/4'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            116171
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        21.547
_diffrn_reflns_theta_max         21.547
_diffrn_reflns_theta_min         1.171
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             4352
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF/H2O'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;                         
The unit cell contains 4 dimethylformamide molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1286
_refine_ls_number_reflns         11823
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0856
_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^)+(0.0431P)^2^+60.2683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9126
_reflns_number_total             11823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04682k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 1548976.cif.'
_cod_original_cell_volume        10261.4(9)
_cod_original_formula_sum        'C58.50 H43.50 F6 N6.50 O2.50 Zn'
_cod_database_code               1548976
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.937
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              78344
_platon_squeeze_void_probe_radius 1.20