Transformations of the cyclo-P4 ligand in [Cp′′′Co(η4-P4)]
Piesch, Martin; Seidl, Michael; Scheer, Manfred; Chemical Science 11 (2020) 6745–6751; doi:10.1039/D0SC01740J

data_1558103
_publ_section_title
;
 Transformations of the cyclo-P4 ligand in
 [Cp&#x2032;&#x2032;&#x2032;Co(\h4-P4)]
;
_journal_issue                   26
_journal_name_full               'Chemical Science'
_journal_page_first              6745
_journal_page_last               6751
_journal_paper_doi               10.1039/D0SC01740J
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C38 H69 Co2 P8 Si, C12 H30 Li O6, C3 H7'
_chemical_formula_sum            'C53 H106 Co2 Li O6 P8 Si'
_chemical_formula_weight         1240.02
_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             2020-01-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-02-17 deposited with the CCDC.	2020-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                102.047(2)
_cell_angle_beta                 94.044(2)
_cell_angle_gamma                114.602(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2675(3)
_cell_length_b                   15.0423(4)
_cell_length_c                   18.2337(5)
_cell_measurement_reflns_used    10597
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.1590
_cell_measurement_theta_min      4.2010
_cell_volume                     3424.69(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.951
_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   -119.00  -8.00   0.50   12.50    --  -40.71 -77.00  30.00  222
  2  \w    -20.00  83.00   0.50   12.50    --   40.71 -99.00 150.00  206
  3  \w    -33.00  70.00   0.50   12.50    --   40.71 -57.00-120.00  206
  4  \w     49.00 153.00   0.50   62.50    --  106.98  15.00  30.00  208
  5  \w     36.00 140.00   0.50   62.50    --  106.98 -77.00 -60.00  208
  6  \w     32.00 121.00   0.50   62.50    --  106.98-125.00 150.00  178
  7  \w     71.00 121.00   0.50   62.50    --  106.98-125.00 -30.00  100
  8  \w     41.00  69.00   0.50   62.50    --  106.98-125.00 -30.00   56
  9  \w     30.00  69.00   0.50   62.50    --  106.98 -30.00 120.00   78
 10  \w     29.00  62.00   0.50   62.50    --  106.98 -30.00  90.00   66
 11  \w     29.00  69.00   0.50   62.50    --  106.98 -30.00   0.00   80
 12  \w     46.00 158.00   0.50   62.50    --  106.98  15.00 -60.00  224
 13  \w     28.00  63.00   0.50   62.50    --  106.98 -94.00  30.00   70
 14  \w     78.00 105.00   0.50   62.50    --  106.98 -94.00  30.00   54
 15  \w     31.00 140.00   0.50   62.50    --  106.98 -77.00 150.00  218
 16  \w   -115.00 -70.00   0.50   12.50    --  -40.71 -57.00  90.00   90
 17  \w   -119.00  -7.00   0.50   12.50    --  -40.71 -77.00-150.00  224
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0288517000
_diffrn_orient_matrix_UB_12      0.0134351000
_diffrn_orient_matrix_UB_13      -0.0786404000
_diffrn_orient_matrix_UB_21      0.0164438000
_diffrn_orient_matrix_UB_22      0.1082198000
_diffrn_orient_matrix_UB_23      0.0379966000
_diffrn_orient_matrix_UB_31      0.1160036000
_diffrn_orient_matrix_UB_32      0.0416504000
_diffrn_orient_matrix_UB_33      -0.0087812000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24262
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.444
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.043
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (Rigaku Oxford Diffraction, 2019)
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 dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       plate
_exptl_crystal_F_000             1326
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         13133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0603P)^2^+1.1649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10990
_reflns_number_total             13133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01740j2.cif
_cod_data_source_block           ap_neu_gaus_CCDC1
_cod_depositor_comments
;Adding full bibliography for 1558098--1558103.cif.

 Adding full bibliography for 1558098--1558103.cif.
;
_cod_original_cell_volume        3424.69(16)
_cod_database_code               1558103
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C53H106Co2LiO6P8Si
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C31(H31A,H31B), C32(H32A,H32B), C35(H35A,H35B), C36(H36A,H36B),
 C39(H39A,H39B), C40(H40A,H40B), C43(H43A,H43B), C44(H44A,H44B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C22(H22), C24(H24)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C101(H10A,H10B,H10C),
 C102(H10D,H10E,H10F), C103(H10G,H10H,H10I), C111(H11A,H11B,H11C), C112(H11D,
 H11E,H11F), C113(H11G,H11H,H11I), C131(H13A,H13B,H13C), C132(H13D,H13E,H13F),
 C133(H13G,H13H,H13I), C201(H20A,H20B,H20C), C202(H20D,H20E,H20F), C203(H20G,
 H20H,H20I), C211(H21A,H21B,H21C), C212(H21D,H21E,H21F), C213(H21G,H21H,H21I),
 C231(H23A,H23B,H23C), C232(H23D,H23E,H23F), C233(H23G,H23H,H23I), C30(H30A,
 H30B,H30C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              75319
_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 1.747
_oxdiff_exptl_absorpt_empirical_full_min 0.615