CO2 reduction by Fe(i): solvent control of C–O cleavage versus C–C coupling
Saouma, Caroline T.; Lu, Connie C.; Day, Michael W.; Peters, Jonas C.; Chemical Science 4 (2013) 4042–; doi:10.1039/c3sc51262b

data_1514558
_publ_section_title
;
 CO2 reduction by Fe(i): solvent control of C--O cleavage versus C--C
 coupling
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              4042
_journal_paper_doi               10.1039/c3sc51262b
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C91 H82 B2 Fe2 O3 P6'
_chemical_formula_weight         1542.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.6650(10)
_cell_angle_beta                 106.7190(10)
_cell_angle_gamma                103.4890(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7605(4)
_cell_length_b                   16.3419(4)
_cell_length_c                   22.5111(6)
_cell_measurement_reflns_used    7260
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      57.55
_cell_measurement_theta_min      2.84
_cell_volume                     4622.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1049
_diffrn_reflns_av_sigmaI/netI    0.1198
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28804
_diffrn_reflns_theta_full        50.44
_diffrn_reflns_theta_max         50.44
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.945
_exptl_absorpt_correction_T_max  0.8908
_exptl_absorpt_correction_T_min  0.2641
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_platon_squeeze_details
; The unit cell contains 8 THF molecules which have been treated as a 
 diffuse contribution to the overall scattering without specific atom 
 positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         9102
_refine_ls_number_restraints     3040
_refine_ls_restrained_S_all      0.797
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                5692
_reflns_number_total             9102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc51262b.txt
_cod_data_source_block           complex15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'const' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1514558