Orientation of Cyano-Substituted Bipyridine Re(I)fac-Tricarbonyl Electrocatalysts Bound to Conducting Au Surfaces
Clark, Melissa L.; Rudshteyn, Benjamin; Ge, Aimin; Chabolla, Steven A.; Machan, Charles W.; Psciuk, Brian T.; Song, Jia; Canzi, Gabriele; Lian, Tianquan; Batista, Victor S.; Kubiak, Clifford P.; The Journal of Physical Chemistry C 120 (2016) 1657–; doi:10.1021/acs.jpcc.5b10912

data_1542290
_publ_section_title
;
 Orientation of Cyano-Substituted Bipyridine Re(I)fac-Tricarbonyl
 Electrocatalysts Bound to Conducting Au Surfaces
;
_journal_issue                   3
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              1657
_journal_paper_doi               10.1021/acs.jpcc.5b10912
_journal_volume                  120
_journal_year                    2016
_chemical_formula_moiety         'C14 H7 Cl N3 O3 Re, C H2 Cl2'
_chemical_formula_sum            'C15 H9 Cl3 N3 O3 Re'
_chemical_formula_weight         571.82
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.538(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7568(8)
_cell_length_b                   11.9888(9)
_cell_length_c                   14.3677(12)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.438
_cell_measurement_theta_min      2.686
_cell_volume                     1756.7(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9899
_diffrn_measured_fraction_theta_max 0.9899
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40655
_diffrn_reflns_theta_full        25.4747
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         3.47
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.393
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0963 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.7550.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.1619
_exptl_crystal_description       block
_exptl_crystal_F_000             1078.8637
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.5997
_refine_diff_density_min         -0.7117
_refine_diff_density_rms         0.1295
_refine_ls_d_res_high            0.8262
_refine_ls_d_res_low             5.8749
_refine_ls_goodness_of_fit_ref   1.0388
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    17
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0388
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0148
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+1.1244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0277
_refine_ls_wR_factor_ref         0.0287
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              -8
_reflns_number_gt                2912
_reflns_number_total             3221
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            jp5b10912_si_003.cif
_cod_data_source_block           kubiak_sc_12_10_14_re_cnbpy_0m
_cod_depositor_comments
'Adding full bibliography for 1542290--1542291.cif.'
_cod_database_code               1542290
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C12(H12), C10(H10), C5(H5), C4(H4), C11(H11), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'