#------------------------------------------------------------------------------
#$Date: 2021-02-05 00:33:17 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261536 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/76/7127612.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7127612
loop_
_publ_author_name
'Greer, Samuel M.'
'Üngor, Ökten'
'Beattie, Ross J.'
'Kiplinger, Jaqueline L.'
'Scott, Brian L.'
'Stein, Benjamin W.'
'Goodwin, Conrad A. P.'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.26 185.26   0.50   10.00    --   28.00  73.75 -25.74  366
  2  ω      2.26 185.26   0.50   10.00    --   28.00  73.75  64.26  366
  3  ω      2.26 185.26   0.50   10.00    --   28.00  73.75 154.26  366
  4  ω      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       'ω 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/[σ²(Fo²)+(0.0306P)²+0.7174P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.500000 0.500000 0.500000 0.01152(13) Uani 1 2 d S T P . .
P1 P 0.64711(6) 0.33269(3) 0.51363(5) 0.01608(13) Uani 1 1 d . . . . .
C1 C 0.7595(2) 0.43632(14) 0.6523(2) 0.0163(4) Uani 1 1 d . . . . .
C2 C 0.7963(2) 0.52871(14) 0.5742(2) 0.0160(3) Uani 1 1 d . . . . .
C3 C 0.7254(2) 0.52055(13) 0.4035(2) 0.0155(3) Uani 1 1 d . . . . .
C4 C 0.6353(2) 0.42172(13) 0.3509(2) 0.0149(3) Uani 1 1 d . . . . .
C5 C 0.8183(2) 0.42210(16) 0.8326(2) 0.0243(4) Uani 1 1 d . . . . .
H5A H 0.816343 0.491174 0.883359 0.036 Uiso 1 1 calc GR . . . .
H5B H 0.941172 0.392922 0.871512 0.036 Uiso 1 1 calc GR . . . .
H5C H 0.735385 0.373029 0.859154 0.036 Uiso 1 1 calc GR . . . .
C6 C 0.8976(2) 0.62519(15) 0.6615(2) 0.0237(4) Uani 1 1 d . . . . .
H6A H 1.026994 0.616726 0.678858 0.036 Uiso 1 1 calc GR . . . .
H6B H 0.878795 0.632173 0.764976 0.036 Uiso 1 1 calc GR . . . .
H6C H 0.852678 0.689139 0.597219 0.036 Uiso 1 1 calc GR . . . .
C7 C 0.7424(3) 0.60793(15) 0.2918(2) 0.0238(4) Uani 1 1 d . . . . .
H7A H 0.868202 0.612482 0.294526 0.036 Uiso 1 1 calc GR . . . .
H7B H 0.706310 0.676023 0.325893 0.036 Uiso 1 1 calc GR . . . .
H7C H 0.663863 0.591856 0.182525 0.036 Uiso 1 1 calc GR . . . .
C8 C 0.5498(2) 0.38995(15) 0.1767(2) 0.0208(4) Uani 1 1 d . . . . .
H8A H 0.470562 0.328405 0.168987 0.031 Uiso 1 1 calc GR . . . .
H8B H 0.644924 0.371326 0.132364 0.031 Uiso 1 1 calc GR . . . .
H8C H 0.478776 0.449610 0.116221 0.031 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Cr1 P1 180.0 . 3_666 ?
C1 Cr1 P1 46.34(5) . . ?
C1 Cr1 P1 133.66(5) . 3_666 ?
C1 Cr1 P1 133.66(5) 3_666 . ?
C1 Cr1 P1 46.34(5) 3_666 3_666 ?
C1 Cr1 C1 180.0 . 3_666 ?
C1 Cr1 C2 142.18(6) . 3_666 ?
C1 Cr1 C2 37.82(6) . . ?
C1 Cr1 C2 142.18(6) 3_666 . ?
C1 Cr1 C2 37.82(6) 3_666 3_666 ?
C1 Cr1 C3 114.64(6) 3_666 . ?
C1 Cr1 C3 65.36(6) . . ?
C1 Cr1 C3 114.64(6) . 3_666 ?
C1 Cr1 C3 65.36(6) 3_666 3_666 ?
C2 Cr1 P1 108.23(5) . 3_666 ?
C2 Cr1 P1 71.77(5) . . ?
C2 Cr1 P1 71.77(5) 3_666 3_666 ?
C2 Cr1 P1 108.23(5) 3_666 . ?
C2 Cr1 C2 180.0 . 3_666 ?
C3 Cr1 P1 108.19(4) 3_666 . ?
C3 Cr1 P1 108.19(4) . 3_666 ?
C3 Cr1 P1 71.81(4) 3_666 3_666 ?
C3 Cr1 P1 71.81(4) . . ?
C3 Cr1 C2 142.45(6) 3_666 . ?
C3 Cr1 C2 37.55(6) 3_666 3_666 ?
C3 Cr1 C2 37.55(6) . . ?
C3 Cr1 C2 142.45(6) . 3_666 ?
C3 Cr1 C3 180.0 . 3_666 ?
C4 Cr1 P1 46.26(4) 3_666 3_666 ?
C4 Cr1 P1 46.26(4) . . ?
C4 Cr1 P1 133.74(4) 3_666 . ?
C4 Cr1 P1 133.74(4) . 3_666 ?
C4 Cr1 C1 109.35(6) . 3_666 ?
C4 Cr1 C1 109.35(6) 3_666 . ?
C4 Cr1 C1 70.65(6) . . ?
C4 Cr1 C1 70.65(6) 3_666 3_666 ?
C4 Cr1 C2 65.27(6) 3_666 3_666 ?
C4 Cr1 C2 114.73(6) 3_666 . ?
C4 Cr1 C2 114.73(6) . 3_666 ?
C4 Cr1 C2 65.27(6) . . ?
C4 Cr1 C3 37.83(6) . . ?
C4 Cr1 C3 142.17(6) 3_666 . ?
C4 Cr1 C3 37.83(6) 3_666 3_666 ?
C4 Cr1 C3 142.17(6) . 3_666 ?
C4 Cr1 C4 180.0 . 3_666 ?
C1 P1 Cr1 61.09(5) . . ?
C4 P1 Cr1 61.09(5) . . ?
C4 P1 C1 88.87(8) . . ?
P1 C1 Cr1 72.58(6) . . ?
C2 C1 Cr1 72.57(9) . . ?
C2 C1 P1 112.80(12) . . ?
C2 C1 C5 124.42(16) . . ?
C5 C1 Cr1 125.96(12) . . ?
C5 C1 P1 122.65(13) . . ?
C1 C2 Cr1 69.61(9) . . ?
C1 C2 C3 112.55(15) . . ?
C1 C2 C6 123.99(16) . . ?
C3 C2 Cr1 71.07(9) . . ?
C3 C2 C6 123.46(16) . . ?
C6 C2 Cr1 126.88(12) . . ?
C2 C3 Cr1 71.38(9) . . ?
C2 C3 C7 123.47(16) . . ?
C4 C3 Cr1 69.73(9) . . ?
C4 C3 C2 112.55(15) . . ?
C4 C3 C7 123.97(15) . . ?
C7 C3 Cr1 126.25(12) . . ?
P1 C4 Cr1 72.65(6) . . ?
C3 C4 Cr1 72.44(9) . . ?
C3 C4 P1 112.97(12) . . ?
C3 C4 C8 124.31(15) . . ?
C8 C4 Cr1 126.50(11) . . ?
C8 C4 P1 122.57(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 P1 2.3813(4) 3_666 ?
Cr1 P1 2.3812(4) . ?
Cr1 C1 2.1846(16) . ?
Cr1 C1 2.1847(16) 3_666 ?
Cr1 C2 2.2236(16) 3_666 ?
Cr1 C2 2.2236(16) . ?
Cr1 C3 2.2196(16) 3_666 ?
Cr1 C3 2.2196(16) . ?
Cr1 C4 2.1840(16) 3_666 ?
Cr1 C4 2.1840(16) . ?
P1 C1 1.8054(18) . ?
P1 C4 1.8024(17) . ?
C1 C2 1.429(2) . ?
C1 C5 1.519(2) . ?
C2 C3 1.430(2) . ?
C2 C6 1.513(2) . ?
C3 C4 1.428(2) . ?
C3 C7 1.514(2) . ?
C4 C8 1.518(2) . ?
