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_7127616
_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         'C14 H17 P'
_chemical_formula_sum            'C14 H17 P'
_chemical_formula_weight         216.24
_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     heavy
_audit_creation_date             2018-01-30
_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                103.1739(17)
_cell_angle_beta                 92.6248(19)
_cell_angle_gamma                100.705(2)
_cell_formula_units_Z            4
_cell_length_a                   8.0727(2)
_cell_length_b                   8.74422(19)
_cell_length_c                   18.4065(4)
_cell_measurement_reflns_used    7494
_cell_measurement_temperature    150.00(1)
_cell_measurement_theta_max      70.8880
_cell_measurement_theta_min      5.0090
_cell_volume                     1237.81(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_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     39.00  71.20   0.70    1.00    --    0.00  14.00-120.00   46
  2  \w    -86.00 -20.90   0.70    1.00    --    0.00  14.00-120.00   93
  3  \w     -1.00  25.60   0.70    1.00    --    0.00  14.00-120.00   38
  4  \w     58.00 142.00   0.70    2.00    --   55.00  60.00 -90.00  120
  5  \w    118.00 142.50   0.70    2.00    --   55.00  43.00   0.00   35
  6  \w      4.00  54.40   0.70    2.00    --   55.00  60.00 -60.00   72
  7  \w      8.00 141.70   0.70    2.00    --   55.00  29.00 -90.00  191
  8  \w    -30.00  -3.40   0.70    2.00    --   55.00  60.00 -90.00   38
  9  \w     52.00  94.70   0.70    2.00    --   55.00  43.00   0.00   61
 10  \w     36.00 143.10   0.70    2.00    --   55.00  60.00 150.00  153
 11  \w     83.00 142.50   0.70    2.00    --   55.00  43.00 150.00   85
 12  \w     39.00  79.60   0.70    2.00    --   55.00  43.00 150.00   58
 13  \w     13.00 143.20   0.70    2.00    --   55.00  60.00  30.00  186
 14  \w    140.00 175.00   0.70    2.00    --  110.00  60.00 120.00   50
 15  \w     88.00 118.10   0.70    2.00    --  110.00  60.00 120.00   43
 16  \w    101.00 133.90   0.70    2.00    --  110.00  29.00-180.00   47
 17  \w     35.00  61.60   0.70    2.00    --  110.00  60.00 120.00   38
 18  \w     81.00 123.00   0.70    2.00    --  110.00  48.00-180.00   60
 19  \w     63.00  89.60   0.70    2.00    --  110.00  48.00  30.00   38
 20  \w     65.00 196.60   0.70    2.00    --  110.00  60.00   0.00  188
 21  \w     35.00 116.20   0.70    2.00    --  110.00  57.00 -60.00  116
 22  \w    100.00 125.90   0.70    2.00    --  110.00  60.00-150.00   37
 23  \w     55.00  80.90   0.70    2.00    --  110.00  38.00 -60.00   37
 24  \w    135.00 160.90   0.70    2.00    --  110.00  48.00  30.00   37
 25  \w    167.00 198.50   0.70    2.00    --  110.00  48.00  30.00   45
 26  \w     22.00  60.50   0.70    2.00    --  110.00  60.00   0.00   55
 27  \w    136.00 194.10   0.70    2.00    --  110.00  60.00  60.00   83
 28  \w     48.00  99.10   0.70    2.00    --  110.00  19.00   0.00   73
 29  \w    131.00 183.50   0.70    2.00    --  110.00  19.00   0.00   75
 30  \w     74.00 165.00   0.70    2.00    --  110.00  60.00-180.00  130
 31  \w     21.00 144.20   0.70    2.00    --  110.00  10.00-180.00  176
 32  \w     88.00 196.50   0.70    2.00    --  110.00  38.00-120.00  155
 33  \w    109.00 186.70   0.70    2.00    --  110.00  57.00-120.00  111
 34  \w     27.00  53.60   0.70    2.00    --  110.00  48.00   0.00   38
 35  \w    119.00 175.00   0.70    2.00    --  110.00  60.00 -30.00   80
 36  \w    133.00 157.50   0.70    2.00    --  110.00  60.00  90.00   35
 37  \w     29.00 117.20   0.70    2.00    --  110.00  60.00  90.00  126
 38  \w     94.00 174.50   0.70    2.00    --  110.00  60.00-120.00  115
 39  \w    125.00 149.50   0.70    2.00    --  110.00  38.00 -90.00   35
 40  \w    154.00 178.50   0.70    2.00    --  110.00   0.00-150.00   35
 41  \w     36.00  61.20   0.70    2.00    --  110.00  10.00 -60.00   36
 42  \w     93.00 118.20   0.70    2.00    --  110.00  10.00 -60.00   36
 43  \w     62.00  87.20   0.70    2.00    --  110.00   0.00-150.00   36
 44  \w    142.00 166.50   0.70    2.00    --  110.00  60.00-150.00   35
 45  \w     57.00  82.20   0.70    2.00    --  110.00  38.00 -90.00   36
 46  \w    146.00 170.50   0.70    2.00    --  110.00  57.00 -60.00   35
 47  \w    163.00 187.50   0.70    2.00    --  110.00  29.00-180.00   35
 48  \w     39.00  64.20   0.70    2.00    --  110.00  57.00-120.00   36
 49  \w     96.00 122.60   0.70    2.00    --  110.00  38.00 -30.00   38
 50  \w    134.00 183.00   0.70    2.00    --  110.00  38.00 -30.00   70
 51  \w    134.00 158.50   0.70    2.00    --  110.00  29.00 -90.00   35
 52  \w     53.00 195.80   0.70    2.00    --  110.00  10.00  30.00  204
 53  \w    133.00 182.70   0.70    2.00    --  110.00  48.00 -30.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1425395000
_diffrn_orient_matrix_UB_12      -0.1132538000
_diffrn_orient_matrix_UB_13      0.0258707000
_diffrn_orient_matrix_UB_21      0.0066191000
_diffrn_orient_matrix_UB_22      0.1263664000
_diffrn_orient_matrix_UB_23      0.0742172000
_diffrn_orient_matrix_UB_31      -0.1329706000
_diffrn_orient_matrix_UB_32      0.0730339000
_diffrn_orient_matrix_UB_33      -0.0357025000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13067
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         2.476
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_recrystallization_method 'Neat compound.'
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0451P)^2^+0.4714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4211
_reflns_number_total             4482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06518h2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7127612--7127619.cif.'
_cod_database_code               7127616
_manchester_internal_coll_name   ldpm35
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 1/2s
_manchester_internal_coll_frame_width 0.7
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   29/1/18
_manchester_internal_process_user CAPG
_manchester_internal_process_date 30/1/18
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 30/1/18
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 30/1/18
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 10/1/2020
_manchester_internal_archive_date 10/1/2020
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         N
_reflns_odcompleteness_completeness 96.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.77
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H5D)=Sof(H5E)=Sof(H5F)=1-FVAR(1)
 Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
 Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
 Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(3)
 Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(3)
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28)
3.b Disordered Me refined with riding coordinates:
 C5(H5A,H5B,H5C,H5D,H5E,H5F), C22(H22A,H22B,H22C,H22D,H22E,H22F), C21(H21A,
 H21B,H21C,H21D,H21E,H21F)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              16833
_shelx_hkl_checksum              74343
_olex2_date_sample_completion    2018-01-29
_olex2_date_sample_data_collection 2018-01-29
_olex2_date_sample_submission    2018-01-29
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_original_sample_id ldpm35
_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 25.031
_oxdiff_exptl_absorpt_empirical_full_min 0.525