Low-spin 1,1'-diphosphametallocenates of chromium and iron.
Greer, Samuel M.; Üngor, Ökten; Beattie, Ross J.; Kiplinger, Jaqueline L.; Scott, Brian L.; Stein, Benjamin W.; Goodwin, Conrad A. P.; Chemical communications (Cambridge, England) 57 (2021) 595–598; doi:10.1039/d0cc06518h

data_7127615
_publ_section_title
;
 Low-spin 1,1'-diphosphametallocenates of chromium and iron.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              595
_journal_page_last               598
_journal_paper_doi               10.1039/d0cc06518h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '2(C8 H12 P), C4 H8 O, 2(C18 H36 K N2 O6)'
_chemical_formula_sum            'C56 H104 K2 N4 O13 P2'
_chemical_formula_weight         1181.57
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2020-07-19 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                64.066(6)
_cell_angle_beta                 85.655(5)
_cell_angle_gamma                86.321(5)
_cell_formula_units_Z            2
_cell_length_a                   12.7189(8)
_cell_length_b                   15.9437(10)
_cell_length_c                   17.8937(12)
_cell_measurement_reflns_used    3339
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      24.5100
_cell_measurement_theta_min      2.0230
_cell_volume                     3251.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      2.27 185.27   0.50   20.00    --   28.00  73.72 -25.73  366
  2  \w      2.27 185.27   0.50   20.00    --   28.00  73.72  64.27  366
  3  \w      2.27 185.27   0.50   20.00    --   28.00  73.72 154.27  366
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0555311000
_diffrn_orient_matrix_UB_12      -0.0013645000
_diffrn_orient_matrix_UB_13      -0.0073585000
_diffrn_orient_matrix_UB_21      0.0037526000
_diffrn_orient_matrix_UB_22      -0.0430916000
_diffrn_orient_matrix_UB_23      0.0360408000
_diffrn_orient_matrix_UB_31      -0.0058233000
_diffrn_orient_matrix_UB_32      -0.0243193000
_diffrn_orient_matrix_UB_33      -0.0243997000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31744
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.993
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From THF.'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1310
_refine_ls_number_reflns         13040
_refine_ls_number_restraints     2121
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0743P)^2^+0.3849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8417
_reflns_number_total             13040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06518h2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7127612--7127619.cif.'
_cod_database_code               7127615
_lanl_internal_coll_name         dq0919
_lanl_internal_coll_client       CAPG
_lanl_internal_coll_type         custom
_lanl_internal_coll_frame_time   20s
_lanl_internal_coll_frame_width  0.5
_lanl_internal_coll_frame_method '\w scans'
_lanl_internal_coll_user         CAPG
_lanl_internal_coll_date         9/27/18
_lanl_internal_process_user      CAPG
_lanl_internal_process_date      9/27/18
_lanl_internal_solution_user     CAPG
_lanl_internal_solution_date     9/28/18
_lanl_internal_refinement_user   CAPG
_lanl_internal_refinement_date   9/28/18
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         KN2O6C18H36PC8H13
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.912
_reflns_odcompleteness_completeness 98.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O13A-C56A \\sim O13A-C53A \\sim O13B-C56B \\sim O13B-C53B
 with sigma of 0.005
 C55B-C54B \\sim C55A-C54A
 with sigma of 0.005
 C56B-C55B \\sim C54B-C53B \\sim C54A-C53A \\sim C56A-C55A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
P2A \\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim
C33A \\sim C34A \\sim P2B \\sim C27B \\sim C28B \\sim C29B \\sim C30B \\sim
C31B \\sim C32B \\sim C33B \\sim C34B: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
K2A \\sim O7A \\sim O8A \\sim O9A \\sim O10A \\sim O11A \\sim O12A \\sim N3A
\\sim N4A \\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39A \\sim C40A
\\sim C41A \\sim C42A \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim C47A
\\sim C48A \\sim C49A \\sim C50A \\sim C51A \\sim C52A \\sim K2B \\sim O7B
\\sim O8B \\sim O9B \\sim O10B \\sim O11B \\sim O12B \\sim N3B \\sim N4B \\sim
C35B \\sim C36B \\sim C37B \\sim C38B \\sim C39B \\sim C40B \\sim C41B \\sim
C42B \\sim C43B \\sim C44B \\sim C45B \\sim C46B \\sim C47B \\sim C48B \\sim
C49B \\sim C50B \\sim C51B \\sim C52B: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.005
O6B \\sim K1B \\sim O1B \\sim O2B \\sim O3B \\sim O5B \\sim O4B \\sim N1B \\sim
N2B \\sim C10B \\sim C11B \\sim C24B \\sim C25B \\sim C12B \\sim C13B \\sim
C16B \\sim C17B \\sim C22B \\sim C23B \\sim C18B \\sim C19B \\sim C9B \\sim
C20B \\sim C21B \\sim C14B \\sim C15B \\sim C26B \\sim C23A \\sim K1A \\sim O1A
\\sim O6A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim N1A \\sim N2A \\sim
C10A \\sim C11A \\sim C24A \\sim C25A \\sim C12A \\sim C13A \\sim C16A \\sim
C17A \\sim C18A \\sim C19A \\sim C22A \\sim C9A \\sim C20A \\sim C21A \\sim
C14A \\sim C15A \\sim C26A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C56A \\sim O13A \\sim C53A \\sim C54A \\sim C55A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.005
C56B \\sim C53B \\sim O13B \\sim C54B \\sim C55B \\sim C55A \\sim O13A \\sim
C53A \\sim C56A \\sim C54A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(P2B)=Sof(C27B)=Sof(C28B)=Sof(C29B)=Sof(C30B)=Sof(C31B)=Sof(H31D)=
 Sof(H31E)=Sof(H31F)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=
 Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(P2A)=Sof(C27A)=Sof(C28A)=Sof(C29A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33A)=
 Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(K2B)=Sof(O7B)=Sof(O8B)=Sof(O9B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=Sof(N3B)=
 Sof(N4B)=Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)=
 Sof(H37C)=Sof(H37D)=Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(C39B)=Sof(H39C)=
 Sof(H39D)=Sof(C40B)=Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=
 Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=
 Sof(H44C)=Sof(H44D)=Sof(C45B)=Sof(H45C)=Sof(H45D)=Sof(C46B)=Sof(H46C)=
 Sof(H46D)=Sof(C47B)=Sof(H47C)=Sof(H47D)=Sof(C48B)=Sof(H48C)=Sof(H48D)=
 Sof(C49B)=Sof(H49C)=Sof(H49D)=Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=
 Sof(H51C)=Sof(H51D)=Sof(C52B)=Sof(H52C)=Sof(H52D)=1-FVAR(2)
 Sof(K2A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(N3A)=
 Sof(N4A)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(C37A)=
 Sof(H37A)=Sof(H37B)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C39A)=Sof(H39A)=
 Sof(H39B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(C41A)=Sof(H41A)=Sof(H41B)=
 Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C44A)=
 Sof(H44A)=Sof(H44B)=Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(C46A)=Sof(H46A)=
 Sof(H46B)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=
 Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(C51A)=
 Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=Sof(H52B)=FVAR(2)
 Sof(K1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(N1B)=
 Sof(N2B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(C11B)=
 Sof(H11A)=Sof(H11B)=Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(C13B)=Sof(H13A)=
 Sof(H13B)=Sof(C14B)=Sof(H14A)=Sof(H14B)=Sof(C15B)=Sof(H15A)=Sof(H15B)=
 Sof(C16B)=Sof(H16A)=Sof(H16B)=Sof(C17B)=Sof(H17A)=Sof(H17B)=Sof(C18B)=
 Sof(H18A)=Sof(H18B)=Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(C20B)=Sof(H20A)=
 Sof(H20B)=Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(C22B)=Sof(H22A)=Sof(H22B)=
 Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(C24B)=Sof(H24A)=Sof(H24B)=Sof(C25B)=
 Sof(H25A)=Sof(H25B)=Sof(C26B)=Sof(H26A)=Sof(H26B)=1-FVAR(3)
 Sof(K1A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(N1A)=
 Sof(N2A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=
 Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15C)=Sof(H15D)=
 Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18A)=
 Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C20A)=Sof(H20C)=
 Sof(H20D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=
 Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C25A)=
 Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=FVAR(3)
 Sof(C53B)=Sof(H53C)=Sof(H53D)=Sof(O13B)=Sof(C56B)=Sof(H56C)=Sof(H56D)=
 Sof(C54B)=Sof(H54C)=Sof(H54D)=Sof(C55B)=Sof(H55C)=Sof(H55D)=1-FVAR(4)
 Sof(O13A)=Sof(C53A)=Sof(H53A)=Sof(H53B)=Sof(C54A)=Sof(H54A)=Sof(H54B)=
 Sof(C55A)=Sof(H55A)=Sof(H55B)=Sof(C56A)=Sof(H56A)=Sof(H56B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C53A(H53A,H53B), C54A(H54A,H54B), C55A(H55A,H55B), C56A(H56A,H56B), C9B(H9BA,
 H9BB), C10B(H10A,H10B), C11B(H11A,H11B), C12B(H12A,H12B), C13B(H13A,H13B),
 C14B(H14A,H14B), C15B(H15A,H15B), C16B(H16A,H16B), C17B(H17A,H17B), C18B(H18A,
 H18B), C19B(H19A,H19B), C20B(H20A,H20B), C21B(H21A,H21B), C22B(H22A,H22B),
 C23B(H23A,H23B), C24B(H24A,H24B), C25B(H25A,H25B), C26B(H26A,H26B), C9A(H9AA,
 H9AB), C10A(H10C,H10D), C11A(H11C,H11D), C12A(H12C,H12D), C13A(H13C,H13D),
 C14A(H14C,H14D), C15A(H15C,H15D), C16A(H16C,H16D), C17A(H17C,H17D), C18A(H18C,
 H18D), C19A(H19C,H19D), C20A(H20C,H20D), C21A(H21C,H21D), C22A(H22C,H22D),
 C23A(H23C,H23D), C24A(H24C,H24D), C25A(H25C,H25D), C26A(H26C,H26D), C35A(H35A,
 H35B), C36A(H36A,H36B), C37A(H37A,H37B), C38A(H38A,H38B), C39A(H39A,H39B),
 C40A(H40A,H40B), C41A(H41A,H41B), C42A(H42A,H42B), C43A(H43A,H43B), C44A(H44A,
 H44B), C45A(H45A,H45B), C46A(H46A,H46B), C47A(H47A,H47B), C48A(H48A,H48B),
 C49A(H49A,H49B), C50A(H50A,H50B), C51A(H51A,H51B), C52A(H52A,H52B), C35B(H35C,
 H35D), C36B(H36C,H36D), C37B(H37C,H37D), C38B(H38C,H38D), C39B(H39C,H39D),
 C40B(H40C,H40D), C41B(H41C,H41D), C42B(H42C,H42D), C43B(H43C,H43D), C44B(H44C,
 H44D), C45B(H45C,H45D), C46B(H46C,H46D), C47B(H47C,H47D), C48B(H48C,H48D),
 C49B(H49C,H49D), C50B(H50C,H50D), C51B(H51C,H51D), C52B(H52C,H52D), C53B(H53C,
 H53D), C56B(H56C,H56D), C54B(H54C,H54D), C55B(H55C,H55D)
5.b Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C31A(H31A,
 H31B,H31C), C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C),
 C31B(H31D,H31E,H31F), C32B(H32D,H32E,H32F), C33B(H33D,H33E,H33F), C34B(H34D,
 H34E,H34F)
;
_shelx_res_checksum              13583
_shelx_hkl_checksum              87602
_olex2_exptl_crystal_mounting_method 'From paratone on a microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.852