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_7127619
_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         'C18 H22 Zr'
_chemical_formula_sum            'C18 H22 Zr'
_chemical_formula_weight         329.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-10
_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                 112.336(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1554(8)
_cell_length_b                   9.6976(4)
_cell_length_c                   12.0182(6)
_cell_measurement_reflns_used    1782
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      26.2880
_cell_measurement_theta_min      3.6050
_cell_volume                     1526.00(15)
_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_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -84.00 -48.00   0.80   30.00    --  -20.40-178.00-150.00   45
  2  \w    -62.00  -2.80   0.80   30.00    --  -20.40 -37.00-180.00   74
  3  \w    -37.00  93.40   0.80   30.00    --   21.65  19.00-150.00  163
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0115250000
_diffrn_orient_matrix_UB_12      -0.0061626000
_diffrn_orient_matrix_UB_13      0.0626350000
_diffrn_orient_matrix_UB_21      0.0314546000
_diffrn_orient_matrix_UB_22      0.0593654000
_diffrn_orient_matrix_UB_23      0.0108000000
_diffrn_orient_matrix_UB_31      -0.0425861000
_diffrn_orient_matrix_UB_32      0.0422089000
_diffrn_orient_matrix_UB_33      -0.0059666000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2872
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.386
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.775
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_recrystallization_method 'From hexane.'
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1558
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0370P)^2^+1.0274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1401
_reflns_number_total             1558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06518h2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7127612--7127619.cif.'
_cod_original_cell_volume        1525.99(14)
_cod_database_code               7127619
_manchester_internal_coll_name   adpm457
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 30s
_manchester_internal_coll_frame_width 0.8
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   9/12/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 9/12/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 9/12/17
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 10/12/17
_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         Zr(C5H5)2(C4(CH3)4)
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C6B)=Sof(H6B)=Sof(C5B)=Sof(H5B)=Sof(C9B)=Sof(H9B)=Sof(C8B)=Sof(H8B)=
 Sof(C7B)=Sof(H7B)=1-FVAR(1)
 Sof(C7A)=Sof(H7A)=Sof(C6A)=Sof(H6A)=Sof(C5A)=Sof(H5A)=Sof(C9A)=Sof(H9A)=
 Sof(C8A)=Sof(H8A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C6A(H6A), C5A(H5A), C9A(H9A), C8A(H8A), C6B(H6B), C5B(H5B),
 C9B(H9B), C8B(H8B), C7B(H7B)
4.b Fitted pentagon refined as free rotating group:
 C7A(C6A,C5A,C9A,C8A), C6B(C5B,C9B,C8B,C7B)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              45155
_shelx_hkl_checksum              3297
_olex2_date_sample_completion    2017-12-09
_olex2_date_sample_data_collection 2017-12-09
_olex2_date_sample_submission    2017-12-09
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_original_sample_id adpm457
_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 1.780
_oxdiff_exptl_absorpt_empirical_full_min 0.658