Bridgehead isomer effects in bis(phosphido)-bridged diiron hexacarbonyl proton reduction electrocatalysts.
Rahaman, Ahibur; Gimbert-Suriñach, Carolina; Ficks, Arne; Ball, Graham E.; Bhadbhade, Mohan; Haukka, Matti; Higham, Lee; Nordlander, Ebbe; Colbran, Stephen B.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3207–3222; doi:10.1039/c6dt01494a

data_7042178
_publ_section_title
;
 Bridgehead isomer effects in bis(phosphido)-bridged diiron hexacarbonyl
 proton reduction electrocatalysts.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3207
_journal_page_last               3222
_journal_paper_doi               10.1039/c6dt01494a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C18 H12 Fe2 O6 P2'
_chemical_formula_sum            'C18 H12 Fe2 O6 P2'
_chemical_formula_weight         497.92
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.111(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2962(6)
_cell_length_b                   14.3680(7)
_cell_length_c                   14.4014(7)
_cell_measurement_reflns_used    8670
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.948
_cell_measurement_theta_min      2.529
_cell_volume                     2013.06(18)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17134
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.565
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1341 before and 0.0382 after correction.
The Ratio of minimum to maximum transmission is 0.8868.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4084
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.2524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3652
_reflns_number_total             4084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01494a2.cif
_cod_data_source_block           74a_yellow_a
_cod_depositor_comments
'Adding full bibliography for 7042178--7042182.cif.'
_cod_database_code               7042178
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C12B(H12B),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B)
;
_shelx_res_checksum              94321
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'