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_7127612
_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 Cr P2'
_chemical_formula_sum            'C16 H24 Cr P2'
_chemical_formula_weight         330.29
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-05
_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                90
_cell_angle_beta                 109.444(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8420(3)
_cell_length_b                   12.5620(4)
_cell_length_c                   8.8611(3)
_cell_measurement_reflns_used    8270
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.3420
_cell_measurement_theta_min      1.6360
_cell_volume                     823.13(5)
_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_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      2.26 185.26   0.50   10.00    --   28.00  73.75 -25.74  366
  2  \w      2.26 185.26   0.50   10.00    --   28.00  73.75  64.26  366
  3  \w      2.26 185.26   0.50   10.00    --   28.00  73.75 154.26  366
  4  \w      2.26 185.26   0.50   10.00    --   28.00  73.75-115.74  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      -0.0416436000
_diffrn_orient_matrix_UB_12      0.0239724000
_diffrn_orient_matrix_UB_13      0.0514157000
_diffrn_orient_matrix_UB_21      0.0861304000
_diffrn_orient_matrix_UB_22      0.0076156000
_diffrn_orient_matrix_UB_23      0.0588678000
_diffrn_orient_matrix_UB_31      0.0067082000
_diffrn_orient_matrix_UB_32      0.0505270000
_diffrn_orient_matrix_UB_33      -0.0331969000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6774
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.928
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80355
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From n-hexane.'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0306P)^2^+0.7174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1441
_reflns_number_total             1508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06518h2.cif
_cod_data_source_block           1-Cr
_cod_depositor_comments
'Adding full bibliography for 7127612--7127619.cif.'
_cod_database_code               7127612
_lanl_internal_coll_name         apx2920
_lanl_internal_coll_client       CAPG
_lanl_internal_coll_type         custom
_lanl_internal_coll_frame_time   00s
_lanl_internal_coll_frame_width  0.5
_lanl_internal_coll_frame_method '\w scans'
_lanl_internal_coll_user         CAPG
_lanl_internal_coll_date         6/3/19
_lanl_internal_process_user      CAPG
_lanl_internal_process_date      6/4/19
_lanl_internal_solution_user     CAPG
_lanl_internal_solution_date     6/4/19
_lanl_internal_refinement_user   CAPG
_lanl_internal_refinement_date   6/5/19
_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         Cr(PC8H12)2
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.710
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              50524
_shelx_hkl_checksum              66289
_olex2_exptl_crystal_mounting_method
'From paratone on a microscope slide, onto a cryoloop.'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.841