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_7042181
_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_absolute_configuration ad
_chemical_formula_moiety         'C48 H32 Fe2 O8 P2'
_chemical_formula_sum            'C48 H32 Fe2 O8 P2'
_chemical_formula_weight         910.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-16
_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                 93.73(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.944(8)
_cell_length_b                   26.47(2)
_cell_length_c                   11.313(11)
_cell_measurement_reflns_used    408
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      18.684
_cell_measurement_theta_min      3.326
_cell_volume                     2374(4)
_computing_cell_refinement       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_collection       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_reduction        '<i>APEX2 </i>(Bruker, 2007)'
_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    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0902
_diffrn_reflns_av_unetI/netI     0.1735
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15590
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.371
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1052 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.5761.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'yellowish orange'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7339
_refine_ls_number_restraints     389
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_gt           0.1106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1894P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2733
_refine_ls_wR_factor_ref         0.2961
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4543
_reflns_number_total             7339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01494a2.cif
_cod_data_source_block           twin_p21
_cod_depositor_comments
'Adding full bibliography for 7042178--7042182.cif.'
_cod_database_code               7042181
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.83(6) 0.17(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O3B-C3B \\sim O3A-C3A \\sim O1B-C1B \\sim O1A-C1A \\sim O2B-C2B \\sim O2A-C2A
 with sigma of 0.02
 Fe1B-C1B \\sim Fe1A-C1A \\sim Fe1A-C3A \\sim Fe1B-C2B \\sim Fe1A-C2A \\sim
Fe1B-C3B
 with sigma of 0.02
 C17B-C18B \\sim C16B-C15B
 with sigma of 0.02
 C28A-C27A \\sim C29A-C28A \\sim C30A-C29A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A)
Uanis(Fe1A) = Uanis(C3A) = Uanis(O3A)
5. Rigid body (RIGU) restrains
 C11B, C12B, H12B, C13B, C14B, C15B, C16B, H16B, C17B, H17B, C18B, C19B, C20B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11B, C21B, C22B, C23B, H23B, C24B, H24B, C25B, H25B, C26B, H26B, C27B, C28B,
 H28B, C29B, H29B, C30B, C32B, H32A, H32B, H32C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11A, C12A, C13A, H13A, C14A, C15A, H15A, C16A, H16A, C17A, C18A, H18A, C19A,
 C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11A, H18A, C21A, C22A, C23A, H23A, C24A, H24A, C25A, H25A, C26A, H26A, C27A,
 C28A, H28A, C29A, H29A, C30A, C31A, H31A, H31B, H31C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3A, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1B, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3B, C3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Fe1A, O2A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 P1A(H1A), P1B(H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C12A(H12A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A),
 C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C28A(H28A), C29A(H29A),
 C12B(H12B), C13B(H13B), C15B(H15B), C16B(H16B), C17B(H17B), C18B(H18B),
 C23B(H23B), C24B(H24B), C25B(H25B), C26B(H26B), C28B(H28B), C29B(H29B)
6.c Fitted hexagon refined as free rotating group:
 C13A(C12A,C11A,C20A,C19A,C14A), C22A(C23A,C24A,C25A,C26A,C27A)
6.d Idealised Me refined as rotating group:
 C31A(H31A,H31B,H31C), C32B(H32A,H32B,H32C)
;
_shelx_res_checksum              60785
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'