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_1558098
_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
'C34 H58 Co2 P8, 2(C18 H36 K N2 O6), 3(C2 H5 O)'
_chemical_formula_sum            'C76 H144 Co2 K2 N4 O15 P8'
_chemical_formula_weight         1797.76
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2020-02-17 deposited with the CCDC.	2020-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                74.8590(10)
_cell_angle_beta                 78.8180(10)
_cell_angle_gamma                65.9260(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7131(2)
_cell_length_b                   15.2042(2)
_cell_length_c                   25.3794(3)
_cell_measurement_reflns_used    18779
_cell_measurement_temperature    123
_cell_measurement_theta_max      72.5670
_cell_measurement_theta_min      4.1320
_cell_volume                     4640.57(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.961
_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    -32.00  71.00   0.50   15.00    --   41.66 -57.00  60.00  206
  2  \w    -32.00  71.00   0.50   15.00    --   41.66 -57.00-180.00  206
  3  \w    -37.00  75.00   0.50   15.00    --   41.66 -77.00 -30.00  224
  4  \w     45.00 178.00   0.50   60.00    --  106.15  15.00-180.00  266
  5  \w     31.00  77.00   0.50   60.00    --  106.15 -45.00  60.00   92
  6  \w     28.00  69.00   0.50   60.00    --  106.15 -30.00 -90.00   82
  7  \w     28.00  69.00   0.50   60.00    --  106.15 -30.00-150.00   82
  8  \w     31.00  77.00   0.50   60.00    --  106.15 -45.00 120.00   92
  9  \w     28.00  69.00   0.50   60.00    --  106.15 -30.00-120.00   82
 10  \w     21.00 145.00   0.50   60.00    --  106.15 -91.00 150.62  248
 11  \w     76.00 178.00   0.50   60.00    --  106.15  61.00-150.00  204
 12  \w     28.00  87.00   0.50   60.00    --  106.15-111.00  30.00  118
 13  \w     31.00  77.00   0.50   60.00    --  106.15 -45.00-180.00   92
 14  \w     21.00 145.00   0.50   60.00    --  106.15 -91.00 -45.29  248
 15  \w     21.00 135.00   0.50   60.00    --  106.15 -91.00  56.28  228
;
_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      -0.0896362000
_diffrn_orient_matrix_UB_12      -0.0064429000
_diffrn_orient_matrix_UB_13      -0.0253721000
_diffrn_orient_matrix_UB_21      -0.0590184000
_diffrn_orient_matrix_UB_22      -0.0170432000
_diffrn_orient_matrix_UB_23      0.0575969000
_diffrn_orient_matrix_UB_31      -0.0614208000
_diffrn_orient_matrix_UB_32      0.1118712000
_diffrn_orient_matrix_UB_33      -0.0057030000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            34504
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.012
_diffrn_reflns_theta_min         3.386
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.379
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         17809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0403P)^2^+1.5570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16566
_reflns_number_total             17809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01740j2.cif
_cod_data_source_block           ap_abs_ana
_cod_depositor_comments
;Adding full bibliography for 1558098--1558103.cif.

 Adding full bibliography for 1558098--1558103.cif.
;
_cod_database_code               1558098
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C34H58Co2P8K(C18N2H36O6)2C4H10O2C2H5O
_chemical_oxdiff_usercomment     'green plate'
_reflns_odcompleteness_completeness 98.98
_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:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
  C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,
 H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C71(H71A,H71B),
 C73(H73A,H73B), C74(H74A,H74B)
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:
 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), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C75(H75A,H75B,H75C)
;
_shelx_res_checksum              1611
_olex2_diffrn_ambient_temperature_device 123
_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 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.747