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_7127614
_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         'C16 H24 Fe P2, C18 H36 K N2 O6'
_chemical_formula_sum            'C34 H60 Fe K N2 O6 P2'
_chemical_formula_weight         749.73
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_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             2018-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2020-05-11 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                62.275(2)
_cell_angle_beta                 85.840(2)
_cell_angle_gamma                87.045(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1947(2)
_cell_length_b                   14.2373(4)
_cell_length_c                   15.0677(3)
_cell_measurement_reflns_used    5215
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      26.1110
_cell_measurement_theta_min      2.4590
_cell_volume                     1930.42(8)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_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   25.00    --   28.00  73.72 -25.73  366
  2  \w      2.27 185.27   0.50   25.00    --   28.00  73.72  64.27  366
  3  \w      2.27 185.27   0.50   25.00    --   28.00  73.72 154.27  366
  4  \w      2.27 185.27   0.50   25.00    --   28.00  73.72-115.73  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      0.0107225000
_diffrn_orient_matrix_UB_12      -0.0512785000
_diffrn_orient_matrix_UB_13      0.0036681000
_diffrn_orient_matrix_UB_21      -0.0302555000
_diffrn_orient_matrix_UB_22      -0.0229433000
_diffrn_orient_matrix_UB_23      0.0491882000
_diffrn_orient_matrix_UB_31      -0.0619514000
_diffrn_orient_matrix_UB_32      0.0036085000
_diffrn_orient_matrix_UB_33      -0.0200929000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25573
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.616
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87191
_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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       plate
_exptl_crystal_F_000             802
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From THF layered with hexane.'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0570P)^2^+0.6123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6351
_reflns_number_total             7807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06518h2.cif
_cod_data_source_block           2-Fe
_cod_depositor_comments
'Adding full bibliography for 7127612--7127619.cif.'
_cod_database_code               7127614
_lanl_internal_coll_name         dq0907
_lanl_internal_coll_client       CAPG
_lanl_internal_coll_type         custom
_lanl_internal_coll_frame_time   25s
_lanl_internal_coll_frame_width  0.5
_lanl_internal_coll_frame_method '\w scans'
_lanl_internal_coll_user         CAPG
_lanl_internal_coll_date         9/12/18
_lanl_internal_process_user      CAPG
_lanl_internal_process_date      9/13/18
_lanl_internal_solution_user     CAPG
_lanl_internal_solution_date     9/13/18
_lanl_internal_refinement_user   CAPG
_lanl_internal_refinement_date   9/13/18
_lanl_internal_validation_user   CAPG
_lanl_internal_validation_date   10/1/2020
_lanl_internal_archive_date      10/1/2020
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Fe(PC8H12)2KN2O6C18H36
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.860
_reflns_odcompleteness_completeness 98.96
_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.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              49908
_shelx_hkl_checksum              18689
_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 1.080
_oxdiff_exptl_absorpt_empirical_full_min 0.915