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_1558099
_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         'C21 H38 Co P4, C18 H36 Li N2 O6, C4 H8 O'
_chemical_formula_sum            'C43 H82 Co Li N2 O7 P4'
_chemical_formula_weight         928.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-15
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8715(3)
_cell_length_b                   22.5218(4)
_cell_length_c                   24.9460(5)
_cell_measurement_reflns_used    5704
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      39.7240
_cell_measurement_theta_min      4.2940
_cell_volume                     10040.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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      5.00 121.00   0.25   25.00    --   39.84  77.00 -30.00  464
  2  \w     32.00 129.00   0.25   25.00    --   39.84-178.00-150.00  388
  3  \w      5.00 121.00   0.25   25.00    --   39.84  77.00-120.00  464
  4  \w      9.00  41.00   0.25   25.00    --   39.84  57.00 120.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0202751000
_diffrn_orient_matrix_UB_12      0.0544070000
_diffrn_orient_matrix_UB_13      -0.0345651000
_diffrn_orient_matrix_UB_21      -0.0107692000
_diffrn_orient_matrix_UB_22      -0.0373095000
_diffrn_orient_matrix_UB_23      -0.0511194000
_diffrn_orient_matrix_UB_31      -0.0830955000
_diffrn_orient_matrix_UB_32      0.0181454000
_diffrn_orient_matrix_UB_33      -0.0018260000
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13776
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        40.147
_diffrn_reflns_theta_max         40.147
_diffrn_reflns_theta_min         3.544
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.248
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       needle
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.665
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         3009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0990P)^2^+2.0268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2723
_reflns_number_total             3009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01740j2.cif
_cod_data_source_block           op_abs_ana
_cod_depositor_comments
;Adding full bibliography for 1558098--1558103.cif.

 Adding full bibliography for 1558098--1558103.cif.
;
_cod_database_code               1558099
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C17H29CoP4C4H9LiC16H32O8
_chemical_oxdiff_usercomment
'flaches braunes Plaettchen, Innenwinkelmessung'
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.164
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     39.54
_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:
 C32(H32A,H32B), C38(H38A,H38B), C33(H33A,H33B), C34(H34A,H34B), C31(H31A,
 H31B), C37(H37A,H37B), C35(H35A,H35B), C39(H39A,H39B), C43(H43A,H43B),
 C41(H41A,H41B), C42(H42A,H42B), C40(H40A,H40B), C36(H36A,H36B), C27(H27A,H27B),
  C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C29(H29A,H29B), C25(H25A,
 H25B), C24(H24A,H24B), C22(H22A,H22B), C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C13(H13A,
 H13B,H13C), C3(H3A,H3B,H3C), C21(H21A,H21B,H21C), C2(H2A,H2B,H2C), C4(H4A,H4B,
 H4C)
;
_shelx_res_checksum              43971
_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 1.716
_oxdiff_exptl_absorpt_empirical_full_min 0.446