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_1558101
_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         'C25 H50 Co Na O5 P4'
_chemical_formula_sum            'C25 H50 Co Na O5 P4'
_chemical_formula_weight         636.45
_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   mixed
_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                78.926(2)
_cell_angle_beta                 89.741(2)
_cell_angle_gamma                85.158(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8103(3)
_cell_length_b                   10.6602(3)
_cell_length_c                   17.7138(5)
_cell_measurement_reflns_used    6889
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      74.1850
_cell_measurement_theta_min      4.1890
_cell_volume                     1626.75(9)
_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      123.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.954
_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    -27.00  67.00   0.50    0.50    --   44.08 -37.00 -60.00  188
  2  \w     33.00  86.00   0.50    2.00    --  104.50 -30.00  30.00  106
  3  \w     82.00 177.00   0.50    2.00    --  104.50  30.00  30.00  190
  4  \w    112.00 176.00   0.50    2.00    --  104.50 125.00 -30.00  128
  5  \w     48.00  91.00   0.50    2.00    --  104.50 -30.00-180.00   86
  6  \w     41.00 141.00   0.50    2.00    --  104.50 -15.00-150.00  200
  7  \w     62.00 117.00   0.50    2.00    --  104.50-125.00 -60.00  110
  8  \w     38.00  99.00   0.50    2.00    --  104.50 -45.00  90.00  122
  9  \w     60.00 121.00   0.50    2.00    --  104.50-125.00 150.00  122
 10  \w     37.00  87.00   0.50    2.00    --  104.50 -45.00   0.00  100
 11  \w     33.00 123.00   0.50    2.00    --  104.50 -77.00 -60.00  180
 12  \w     21.00 115.00   0.50    0.50    --   44.08  37.00 120.00  188
 13  \w   -130.00 -42.00   0.50    0.50    --  -44.08 178.00  90.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0430612000
_diffrn_orient_matrix_UB_12      -0.0392117000
_diffrn_orient_matrix_UB_13      0.0851544000
_diffrn_orient_matrix_UB_21      -0.1427982000
_diffrn_orient_matrix_UB_22      -0.0572358000
_diffrn_orient_matrix_UB_23      -0.0241783000
_diffrn_orient_matrix_UB_31      0.0924886000
_diffrn_orient_matrix_UB_32      -0.1304965000
_diffrn_orient_matrix_UB_33      0.0043272000
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10786
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.291
_diffrn_reflns_theta_min         2.542
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.376
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.226
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0823P)^2^+0.0929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6143
_reflns_number_total             6333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01740j2.cif
_cod_data_source_block           ap_neu_gaus
_cod_depositor_comments
;Adding full bibliography for 1558098--1558103.cif.

 Adding full bibliography for 1558098--1558103.cif.
;
_cod_database_code               1558101
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H50CoNaO5P4
_shelx_estimated_absorpt_t_max   0.465
_shelx_estimated_absorpt_t_min   0.138
_reflns_odcompleteness_completeness 99.60
_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:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), 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)
;
_shelx_res_checksum              91411
_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 3.531
_oxdiff_exptl_absorpt_empirical_full_min 0.443