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_1558100
_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
'C50 H91 Co2 Li O3 P8, 0.5(C5 H12), 0.25(C4 H8 O)'
_chemical_formula_sum            'C53.5 H99 Co2 Li O3.25 P8'
_chemical_formula_weight         1166.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-17
_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                 91.670(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.947(3)
_cell_length_b                   15.5710(12)
_cell_length_c                   12.6636(10)
_cell_measurement_reflns_used    4268
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.0260
_cell_measurement_theta_min      3.5380
_cell_volume                     6296.8(9)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5096
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_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    -98.00  13.00   0.25   40.00    --  -19.91 -77.00-150.00  444
  2  \w    -51.00  54.00   0.25   40.00    --  -19.91  57.00  60.00  420
;
_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      -0.0001553000
_diffrn_orient_matrix_UB_12      0.0439042000
_diffrn_orient_matrix_UB_13      0.0151227000
_diffrn_orient_matrix_UB_21      -0.0067969000
_diffrn_orient_matrix_UB_22      -0.0117325000
_diffrn_orient_matrix_UB_23      0.0508739000
_diffrn_orient_matrix_UB_31      0.0211283000
_diffrn_orient_matrix_UB_32      -0.0034971000
_diffrn_orient_matrix_UB_33      0.0182782000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1458
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19403
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.156
_diffrn_reflns_theta_max         25.156
_diffrn_reflns_theta_min         3.242
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.849
_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)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.250
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         19403
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0745
_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^)+(0.0920P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9021
_reflns_number_total             19403
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9992\% 
 around [-0.00 -0.00 1.00] (reciprocal) or [0.01 0.00 1.00] (direct)
;
_cod_data_source_file            d0sc01740j2.cif
_cod_data_source_block           mp_twin_837_abs_twin1_hklf4
_cod_depositor_comments
;Adding full bibliography for 1558098--1558103.cif.

 Adding full bibliography for 1558098--1558103.cif.
;
_cod_original_formula_sum        'C53.50 H99 Co2 Li O3.25 P8'
_cod_database_code               1558100
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C52H96Co2LiO3.5P8
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.791
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5027(12)
 0.4973(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O5-C57 = O5-C60
 1.45 with sigma of 0.01
 C55-C56 = C52-C53 = C54-C55 = C54-C53
 1.55 with sigma of 0.02
 C58-C57 = C59-C58 = C60-C59
 1.5 with sigma of 0.02
 C60-C57
 2.3 with sigma of 0.02
 O5-C58 \\sim O5-C59
 with sigma of 0.04
 C56-C54 \\sim C54-C52
 with sigma of 0.04
 C58-C60 \\sim C57-C59
 with sigma of 0.04
 C17B-C14 \\sim C17A-C14 \\sim C15-C14 \\sim C16A-C14 \\sim C16B-C14
 with sigma of 0.02
 C49B-C48 \\sim C49A-C48 \\sim C50B-C49B \\sim C50A-C49A \\sim C50A-C51 \\sim
C50B-C51
 with sigma of 0.02
 C46B-C47B \\sim C46A-C47A \\sim C46B-C45 \\sim C46A-C45 \\sim C45-C44
 with sigma of 0.02
 O3-C47A \\sim O3-C47B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C54 \\sim C56 \\sim C55 \\sim C53 \\sim C52: within 1.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.8A
O5 \\sim C60 \\sim C57 \\sim C58 \\sim C59: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
C16A \\sim C14 \\sim C16B \\sim C4 \\sim C17B \\sim C17A: within 1.9A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.9A
C50A \\sim C50B \\sim C49A \\sim C49B \\sim C48 \\sim C51: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C47A \\sim C47B \\sim C46B \\sim C46A \\sim C45 \\sim C44 \\sim O3: within 1.8A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.8A
5. Others
 Fixed Sof: H48A(0.5) H48B(0.5) H48C(0.5) H48D(0.5) C47A(0.4) H47A(0.4)
 H47B(0.4) H51A(0.5) H51B(0.5) H51C(0.5) H51D(0.5) C49A(0.5) H49A(0.5)
 H49B(0.5) H45A(0.4) H45B(0.4) H45C(0.6) H45D(0.6) C46A(0.4) H46A(0.4)
 H46B(0.4) C50A(0.5) H50A(0.5) H50B(0.5) C16B(0.5) H16A(0.5) H16B(0.5)
 H16C(0.5) C17B(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C17A(0.5) H17D(0.5)
 H17E(0.5) H17F(0.5) C16A(0.5) H16D(0.5) H16E(0.5) H16F(0.5) C54(0.5) H54A(0.5)
 H54B(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C55(0.5) H55A(0.5) H55B(0.5)
 C53(0.5) H53A(0.5) H53B(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C50B(0.5)
 H50C(0.5) H50D(0.5) C49B(0.5) H49C(0.5) H49D(0.5) C47B(0.6) H47C(0.6)
 H47D(0.6) C46B(0.6) H46C(0.6) H46D(0.6) O5(0.25) C57(0.25) H57A(0.25)
 H57B(0.25) C58(0.25) H58A(0.25) H58B(0.25) C59(0.25) H59A(0.25) H59B(0.25)
 C60(0.25) H60A(0.25) H60B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C43(H43A,H43B), C41(H41A,H41B), C44(H44A,H44B), C42(H42A,
 H42B), C48(H48A,H48B), C48(H48C,H48D), C47A(H47A,H47B), C51(H51A,H51B),
 C51(H51C,H51D), C49A(H49A,H49B), C45(H45A,H45B), C45(H45C,H45D), C46A(H46A,
 H46B), C50A(H50A,H50B), C54(H54A,H54B), C55(H55A,H55B), C53(H53A,H53B),
 C50B(H50C,H50D), C49B(H49C,H49D), C47B(H47C,H47D), C46B(H46C,H46D), C57(H57A,
 H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C22(H22), C20(H20)
6.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C7(H7A,H7B,H7C), C24(H24A,H24B,H24C), C12(H12A,H12B,
 H12C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C13(H13A,H13B,H13C), C29(H29A,
 H29B,H29C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C11(H11A,H11B,H11C),
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C36(H36A,H36B,H36C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C15(H15A,H15B,
 H15C), C16B(H16A,H16B,H16C), C17B(H17A,H17B,H17C), C17A(H17D,H17E,H17F),
 C16A(H16D,H16E,H16F), C56(H56A,H56B,H56C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              84319
_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 1.363
_oxdiff_exptl_absorpt_empirical_full_min 0.804
_oxdiff_exptl_absorpt_spherical_max 0.910
_oxdiff_exptl_absorpt_spherical_min 0.910
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2