Multi-phosphine-chelated iron-carbide clusters <i>via</i> redox-promoted ligand exchange on an inert hexa-iron-carbide carbonyl cluster, [Fe<sub>6</sub>(μ<sub>6</sub>-C)(μ<sub>2</sub>-CO)<sub>4</sub>(CO)<sub>12</sub>]<sup>2</sup>.
Cobb, Caitlyn R.; Ngo, Ren K.; Dick, Emily J.; Lynch, Vincent M.; Rose, Michael J.; Chemical science 15 (2024) 11455–11471; doi:10.1039/d4sc01370k

data_1571968
_publ_section_title
;
 Multi-phosphine-chelated iron-carbide clusters <i>via</i> redox-promoted
 ligand exchange on an inert hexa-iron-carbide carbonyl cluster,
 [Fe<sub>6</sub>(&#x3bc;<sub>6</sub>-C)(&#x3bc;<sub>2</sub>-CO)<sub>4</sub>(CO)<sub>12</sub>]<sup>2</sup>.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11455
_journal_page_last               11471
_journal_paper_doi               10.1039/d4sc01370k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C43 H33 Fe3 O8 P3), 3(C7 H8)'
_chemical_formula_sum            'C107 H90 Fe6 O16 P6'
_chemical_formula_weight         2152.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-02 deposited with the CCDC.	2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                101.231(5)
_cell_angle_beta                 99.701(5)
_cell_angle_gamma                104.279(5)
_cell_formula_units_Z            2
_cell_length_a                   10.0809(6)
_cell_length_b                   20.0100(11)
_cell_length_c                   25.3574(12)
_cell_measurement_reflns_used    5732
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      51.8880
_cell_measurement_theta_min      4.5990
_cell_volume                     4734.3(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.760
_diffrn_measured_fraction_theta_max 0.760
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 0.760
_diffrn_reflns_Laue_measured_fraction_max 0.760
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14550
_diffrn_reflns_point_group_measured_fraction_full 0.760
_diffrn_reflns_point_group_measured_fraction_max 0.760
_diffrn_reflns_theta_full        51.952
_diffrn_reflns_theta_max         51.952
_diffrn_reflns_theta_min         4.591
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.695
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.58721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       needle
_exptl_crystal_F_000             2212
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.937
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1271
_refine_ls_number_reflns         8051
_refine_ls_number_restraints     433
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1114P)^2^+45.3231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2349
_refine_ls_wR_factor_ref         0.2546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5745
_reflns_number_total             8051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01370k3.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 1571968--1571976.cif.'
_cod_database_code               1571968
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Shared sites
{C1A, H03I}
2. Others
 Fixed Uiso: H00R(0.074) H00S(0.046) H00V(0.049) H00X(0.065) H00A(0.048)
 H00B(0.048) H00Z(0.057) H010(0.063) H014(0.067) H017(0.073) H018(0.055)
 H019(0.075) H01A(0.069) H01B(0.074) H01L(0.063) H01M(0.068) H01E(0.07)
 H01F(0.055) H01G(0.062) H01N(0.069) H01I(0.058) H01J(0.053) H01P(0.057)
 H01C(0.055) H01D(0.055) H01Q(0.072) H01O(0.077) H01R(0.066) H01S(0.051)
 H01T(0.051) H01X(0.063) H01Y(0.058) H01H(0.05) H01K(0.05) H02C(0.053)
 H02D(0.053) H023(0.076) H025(0.066) H02A(0.044) H02B(0.044) H027(0.06)
 H028(0.062) H029(0.064) H02F(0.065) H02G(0.076) H02H(0.069) H02E(0.07)
 H02I(0.068) H02K(0.061) H02J(0.065) H02N(0.071) H02L(0.078) H02M(0.071)
 H02O(0.075) H02P(0.065) H02Q(0.069) H02R(0.068) H02S(0.063) H02T(0.055)
 H02U(0.055) H02V(0.062) H02W(0.068) H02Y(0.069) H03A(0.057) H03B(0.057)
 H033(0.077) H038(0.07) H03I(0.071) H02Z(0.069) H03L(0.069) H035(0.067)
 H03C(0.11) H03D(0.105) H03E(0.12) H03F(0.117) H03M(0.183) H03N(0.183)
 H03O(0.183) H03H(0.113) H03P(0.146) H03G(0.244) H03J(0.244) H03K(0.244)
 H03Q(0.158) H03R(0.163) H03S(0.164) HNT2(0.143) H1A(0.099) H1B(0.099)
 H1C(0.099) H1AA(0.1) H1AB(0.1) H1AC(0.1) H3(0.069) H02{(0.071) H4(0.07)
 H5(0.072) H6(0.069)
 Fixed X: H00R(0.804585) H00S(0.502552) H00V(0.237982) H00X(0.763475) H00A(-
 0.008174) H00B(0.101529) H00Z(0.145404) H010(0.214395) H014(0.674942)
 H017(0.164642) H018(0.53037) H019(0.242546) H01A(0.871929) H01B(0.979729)
 H01L(0.219742) H01M(0.344141) H01E(0.800812) H01F(0.83913) H01G(0.804777)
 H01N(-0.048951) H01I(0.865588) H01J(0.75706) H01P(0.145566) H01C(0.924184)
 H01D(0.962061) H01Q(0.129714) H01O(1.009567) H01R(0.324703) H01S(0.079199)
 H01T(0.111447) H01X(0.532155) H01Y(0.866008) H01H(0.904068) H01K(1.010584)
 H02C(0.030033) H02D(0.059367) H023(0.466707) H025(0.756774) H02A(0.91152)
 H02B(0.945022) H027(0.600418) H028(0.702789) H029(0.520069) H02F(0.150511)
 H02G(0.042803) H02H(0.067947) H02E(0.561376) H02I(0.289727) H02K(0.354425)
 H02J(0.535007) H02N(0.502005) H02L(0.465254) H02M(0.843056) H02O(0.58892)
 H02P(0.482553) H02Q(0.472976) H02R(0.503267) H02S(0.506269) H02T(0.110208)
 H02U(0.224312) H02V(0.398064) H02W(0.442109) H02Y(0.59258) H03A(0.750151)
 H03B(0.860656) H033(0.437033) H038(0.031917) H03I(-0.150903) H02Z(-0.182412)
 H03L(-0.031102) H035(0.18323) H03C(-0.172818) H03D(0.09256) H03E(-0.113026)
 H03F(-0.230462) H03M(0.998381) H03N(0.8691) H03O(0.85502) H03H(0.164607)
 H03P(0.790432) H03G(0.13762) H03J(0.065846) H03K(-0.022857) H03Q(1.237182)
 H03R(0.852683) H03S(1.069878) HNT2(1.170654) H1A(0.249285) H1B(0.235304)
 H1C(0.124438) H1AA(-0.113003) H1AB(-0.235856) H1AC(-0.164028) H3(0.075193)
 H02{(0.240671) H4(0.221783) H5(0.047023) H6(-0.124411)
 Fixed Y: H00R(0.630617) H00S(0.1036) H00V(-0.005259) H00X(0.613435)
 H00A(0.094977) H00B(0.065785) H00Z(0.121739) H010(-0.121453) H014(0.145524)
 H017(-0.157653) H018(0.417466) H019(0.434199) H01A(0.141889) H01B(0.049447)
 H01L(0.316898) H01M(0.353922) H01E(0.076673) H01F(0.431115) H01G(0.197018)
 H01N(0.393125) H01I(0.483273) H01J(0.503774) H01P(0.039969) H01C(0.297669)
 H01D(0.365267) H01Q(-0.079065) H01O(0.07856) H01R(-0.023232) H01S(0.167735)
 H01T(0.213606) H01X(0.248255) H01Y(0.387724) H01H(0.443593) H01K(0.41011)
 H02C(0.11326) H02D(0.185156) H023(0.431311) H025(0.097551) H02A(0.298153)
 H02B(0.355924) H027(0.241566) H028(0.545569) H029(0.269405) H02F(0.030578)
 H02G(0.452905) H02H(0.32301) H02E(0.056152) H02I(0.417572) H02K(0.240601)
 H02J(0.511601) H02N(0.428602) H02L(-0.006878) H02M(0.53941) H02O(0.349461)
 H02P(0.486794) H02Q(0.170186) H02R(0.178571) H02S(0.013949) H02T(0.207997)
 H02U(0.164802) H02V(0.423961) H02W(0.30163) H02Y(0.085748) H03A(0.312)
 H03B(0.266706) H033(0.053473) H038(0.315463) H03I(0.325907) H02Z(0.272053)
 H03L(0.207756) H035(0.251164) H03C(0.011638) H03D(0.233912) H03E(0.223201)
 H03F(0.109739) H03M(0.657267) H03N(0.593063) H03O(0.634623) H03H(0.135648)
 H03P(0.487947) H03G(0.016445) H03J(-0.025122) H03K(-0.031424) H03Q(0.547981)
 H03R(0.406329) H03S(0.431771) HNT2(0.632669) H1A(0.206599) H1B(0.167779)
 H1C(0.135322) H1AA(0.369237) H1AB(0.297282) H1AC(0.312203) H3(0.299899)
 H02{(0.243319) H4(0.187407) H5(0.195835) H6(0.249352)
 Fixed Z: H00R(0.682191) H00S(1.083698) H00V(0.979801) H00X(0.586884)
 H00A(0.973235) H00B(1.009258) H00Z(1.131136) H010(0.934612) H014(0.462169)
 H017(0.839892) H018(0.416843) H019(1.056939) H01A(0.612841) H01B(0.476367)
 H01L(1.093109) H01M(1.014671) H01E(0.422578) H01F(0.666588) H01G(0.400311)
 H01N(0.914728) H01I(0.316111) H01J(0.531145) H01P(0.829831) H01C(0.56641)
 H01D(0.61748) H01Q(0.78779) H01O(0.572957) H01R(1.17436) H01S(1.067775)
 H01T(1.023362) H01X(1.166754) H01Y(0.355721) H01H(0.496206) H01K(0.529313)
 H02C(0.87242) H02D(0.918463) H023(1.242271) H025(0.325695) H02A(0.465612)
 H02B(0.429794) H027(0.6815) H028(0.326326) H029(0.314588) H02F(1.175015)
 H02G(1.008364) H02H(0.870832) H02E(0.57234) H02I(1.16722) H02K(0.794729)
 H02J(0.375788) H02N(0.75819) H02L(0.632228) H02M(0.723246) H02O(1.241339)
 H02P(0.84367) H02Q(0.24067) H02R(0.739742) H02S(1.13086) H02T(0.836816)
 H02U(0.840278) H02V(0.904134) H02W(0.734463) H02Y(0.245743) H03A(0.6439)
 H03B(0.647256) H033(0.715071) H038(0.166382) H03I(0.210358) H02Z(0.283177)
 H03L(0.31202) H035(0.195226) H03C(0.725543) H03D(0.719979) H03E(0.752027)
 H03F(0.761589) H03M(1.272131) H03N(1.273661) H03O(1.226047) H03H(0.690649)
 H03P(1.200416) H03G(0.671112) H03J(0.711684) H03K(0.651397) H03Q(1.163124)
 H03R(1.137319) H03S(1.116654) HNT2(1.223502) H1A(0.310079) H1B(0.247093)
 H1C(0.280452) H1AA(0.23858) H1AB(0.229947) H1AC(0.180085) H3(0.181261)
 H02{(0.209878) H4(0.281377) H5(0.330615) H6(0.299584)
;
_shelx_res_checksum              23416
_olex2_submission_special_instructions 'No special instructions were received'