Intramolecular hydrogen-bonding in a cobalt aqua complex and electrochemical water oxidation activity.
Khosrowabadi Kotyk, Juliet F.; Hanna, Caitlin M.; Combs, Rebecca L.; Ziller, Joseph W.; Yang, Jenny Y.; Chemical science 9 (2018) 2750–2755; doi:10.1039/c7sc04960a

data_1548881
_publ_section_title
;
 Intramolecular hydrogen-bonding in a cobalt aqua complex and
 electrochemical water oxidation activity.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2750
_journal_page_last               2755
_journal_paper_doi               10.1039/c7sc04960a
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_sum            'C20 H28 B2 Co F8 N6'
_chemical_formula_weight         585.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-17 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8793(6)
_cell_length_b                   14.9748(8)
_cell_length_c                   17.3244(10)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.92
_cell_measurement_theta_min      2.35
_cell_volume                     2563.0(3)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker SMART 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  0.0238
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30266
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.003
_diffrn_reflns_theta_min         1.798
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.9622
_exptl_absorpt_correction_T_min  0.8095
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
; 
A yellow crystal of approximate dimensions 0.167 x 0.256 x 0.311 mm was mounted on a glass fiber 
and transferred to a Bruker SMART APEX II diffractometer.  The APEX2 program package was used to 
determine the unit-cell parameters and for data collection (20 sec/frame scan time for a sphere of 
diffraction data).  The raw frame data was processed using SAINT and SADABS to yield the reflection 
data file.  Subsequent calculations were carried out using the SHELXTL program.  The diffraction 
symmetry was mmm and the systematic absences were consistent with the orthorhombic space group P212121 
that was later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix least-squares techniques.  
The analytical scattering factors for neutral atoms were used throughout the analysis.  Hydrogen atoms 
were located from a difference-Fourier map and refined (x,y,z and Uiso). 

At convergence, wR2 = 0.0569 and Goof = 1.023 for 447 variables refined against 6415 data (0.73\%A), 
R1 = 0.0235 for those 6003 data with I > 2.0sigma(I).  The structure was refined as a two-component 
inversion twin.
;
_refine_ls_abs_structure_Flack   0.439(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         6415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0316P)^2^+0.5278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                6033
_reflns_number_total             6415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04960a2.cif
_cod_data_source_block           jyy12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1548879--1548882.cif.
;
_cod_database_code               1548881
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.800
_shelx_estimated_absorpt_t_max   0.885
_shelx_res_checksum              36122