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_1542291
_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         'C15 H6 Cl N4 O3 Re, C H2 Cl2'
_chemical_formula_sum            'C16 H8 Cl3 N4 O3 Re'
_chemical_formula_weight         596.83
_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                 100.728(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3755(10)
_cell_length_b                   11.7615(14)
_cell_length_c                   19.164(2)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.51
_cell_volume                     1854.8(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9873
_diffrn_measured_fraction_theta_max 0.9873
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0401
_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       -27
_diffrn_reflns_number            20925
_diffrn_reflns_theta_full        30.6644
_diffrn_reflns_theta_max         30.66
_diffrn_reflns_theta_min         2.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.009
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1119 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.7104.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.1371
_exptl_crystal_description       block
_exptl_crystal_F_000             1126.8610
_exptl_crystal_preparation
'slow evaporation of supersaturated solution of dichloromethane'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.8592
_refine_diff_density_min         -0.8421
_refine_diff_density_rms         0.1912
_refine_ls_d_res_high            0.6968
_refine_ls_d_res_low             9.4146
_refine_ls_goodness_of_fit_ref   1.0383
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    15
_refine_ls_number_parameters     243
_refine_ls_number_reflns         5661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0383
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+0.7328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0518
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -9
_reflns_number_gt                5074
_reflns_number_total             5661
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            jp5b10912_si_002.cif
_cod_data_source_block           Kubiak_MLC_150105_Redi_0m
_cod_depositor_comments
'Adding full bibliography for 1542290--1542291.cif.'
_cod_database_code               1542291
_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:
 C16(H16a,H16b)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C13(H13), C12(H12), C10(H10)
;
_olex2_date_sample_submission    'January 5, 2015'
_olex2_submission_special_instructions 'No special instructions were received'