Construction of Alkyl-Substituted Pentaphosphido Ligands in the Coordination Sphere of Cobalt
Ziegler, Christoph G. P.; Maier, Thomas M.; Pelties, Stefan; Taube, Clemens; Hennersdorf, Felix; Ehlers, A.W.; Weigand, Jan J.; Wolf, Robert; Chemical Science  (2019) –; doi:10.1039/C8SC04745F

data_1550324
_publ_section_title
;
 Construction of Alkyl-Substituted Pentaphosphido Ligands in the
 Coordination Sphere of Cobalt
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04745F
_journal_year                    2019
_chemical_formula_moiety         'C38 H40 Co N2, C16 H40 K O8'
_chemical_formula_sum            'C54 H80 Co K N2 O8'
_chemical_formula_weight         983.23
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2018-08-13 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                105.4393(15)
_cell_angle_beta                 90.5348(15)
_cell_angle_gamma                90.8565(17)
_cell_formula_units_Z            8
_cell_length_a                   15.3646(3)
_cell_length_b                   25.7695(5)
_cell_length_c                   27.6375(4)
_cell_measurement_reflns_used    27392
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4410
_cell_measurement_theta_min      3.8660
_cell_volume                     10545.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
  1 omega  -68.00   28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9797   37.0000   60.0000 96

  2 omega -116.00  -20.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9797  -37.0000 -120.0000 96

  3 omega  -20.00   83.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.9797  -99.0000  150.0000 103

  4 omega   31.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 100

  5 omega   31.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -150.0000 100

  6 omega   21.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  120.0000 88

  7 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000   30.0000 100

  8 omega   21.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000   30.0000 88

  9 omega   30.00  136.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000 -150.0000 106

 10 omega   31.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -30.0000 100

 11 omega -114.00  -18.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9797  -57.0000 -180.0000 96

 12 omega -114.00  -18.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9797  -57.0000    0.0000 96

 13 omega -114.00  -18.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9797  -57.0000   90.0000 96

 14 omega   80.00  175.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000 -150.0000 95

 15 omega   65.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000  -60.0000 113

 16 omega   73.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   77.0000   60.0000 105

 17 omega   73.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   77.0000  150.0000 105

 18 omega   73.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   77.0000  -60.0000 105

 19 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000  150.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0304036000
_diffrn_orient_matrix_UB_12      0.0444356000
_diffrn_orient_matrix_UB_13      0.0465561000
_diffrn_orient_matrix_UB_21      -0.0603236000
_diffrn_orient_matrix_UB_22      0.0402095000
_diffrn_orient_matrix_UB_23      -0.0154862000
_diffrn_orient_matrix_UB_31      -0.0741236000
_diffrn_orient_matrix_UB_32      -0.0160151000
_diffrn_orient_matrix_UB_33      0.0306183000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            135248
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         73.602
_diffrn_reflns_theta_min         3.321
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.678
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             4224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DME/n-hexane'
_exptl_crystal_size_max          0.1887
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.0838
_refine_diff_density_max         1.536
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2479
_refine_ls_number_reflns         41065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0710
_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^)+(0.0927P)^2^+14.1304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.1999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29362
_reflns_number_total             41065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04745f2.cif
_cod_data_source_block           1_[K(dme)][(MesBIAN)Co(cod)]
_cod_original_cell_volume        10545.7(4)
_cod_database_code               1550324
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C432  H640  Co8  K8  N16  O64  '
_reflns_odcompleteness_completeness 99.27
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O18(0.61902) C147(0.61902) H14G(0.61902) H14H(0.61902)
 H14I(0.61902) C148(0.61902) H14J(0.61902) H14K(0.61902) H14L(0.59383)
 H14M(0.59383) H14N(0.40617) H14O(0.40617) C94(0.61303) H94A(0.61303)
 H94B(0.61303) C95(0.61303) H95A(0.61303) H95B(0.61303) O18A(0.38098)
 C95A(0.38697) H95C(0.38697) H95D(0.38697) C94A(0.38697) H94C(0.38697)
 H94D(0.38697) C1A(0.38098) H1AA(0.38098) H1AB(0.38098) C1B(0.38098)
 H1BA(0.38098) H1BB(0.38098) H1BC(0.38098)
3.a Ternary CH refined with riding coordinates:
 C32(H32), C33(H33), C36(H36), C37(H37), C140(H140), C141(H141), C144(H144),
 C145(H145), C86(H86), C87(H87), C90(H90), C91(H91), C194(H194), C195(H195),
 C198(H198), C199(H199)
3.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C34(H34A,H34B), C35(H35A,H35B), C38(H38A,H38B), C139(H13J,
 H13K), C142(H14A,H14B), C143(H14C,H14D), C146(H14E,H14F), C85(H85A,H85B),
 C88(H88A,H88B), C89(H89A,H89B), C92(H92A,H92B), C193(H19M,H19N), C196(H19O,
 H19P), C197(H19Q,H19R), C200(H20D,H20E), C40(H40A,H40B), C41(H41A,H41B),
 C44(H44A,H44B), C45(H45A,H45B), C48(H48A,H48B), C49(H49A,H49B), C52(H52A,H52B),
  C53(H53A,H53B), C148(H14J,H14K), C149(H14L,H14M), C149(H14N,H14O), C152(H15G,
 H15H), C153(H15I,H15J), C156(H15Q,H15R), C157(H15S,H15T), C160(H16A,H16B),
 C161(H16C,H16D), C94(H94A,H94B), C95(H95A,H95B), C99(H99A,H99B), C100(H10A,
 H10B), C101(H10C,H10D), C105(H10N,H10O), C106(H10P,H10Q), C108(H10U,H10V),
 C202(H20I,H20J), C203(H20K,H20L), C206(H20S,H20T), C207(H20U,H20V), C210(H21D,
 H21E), C211(H21F,H21G), C214(H21N,H21O), C215(H21P,H21Q), C95A(H95C,H95D),
 C94A(H94C,H94D), C1A(H1AA,H1AB)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C15(H15), C17(H17),
 C24(H24), C26(H26), C112(H112), C113(H113), C114(H114), C116(H116), C117(H117),
  C118(H118), C123(H123), C125(H125), C132(H132), C134(H134), C58(H58),
 C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C69(H69), C71(H71), C78(H78),
  C80(H80), C166(H166), C167(H167), C168(H168), C170(H170), C171(H171),
 C172(H172), C177(H177), C179(H179), C186(H186), C188(H188)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C127(H12A,H12B,H12C),
 C128(H12D,H12E,H12F), C129(H12G,H12H,H12I), C136(H13A,H13B,H13C), C137(H13D,
 H13E,H13F), C138(H13G,H13H,H13I), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C),
 C75(H75A,H75B,H75C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,
 H84C), C181(H18A,H18B,H18C), C182(H18D,H18E,H18F), C183(H18G,H18H,H18I),
 C190(H19D,H19E,H19F), C191(H19G,H19H,H19I), C192(H19J,H19K,H19L), C39(H39A,
 H39B,H39C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C54(H54A,H54B,
 H54C), C147(H14G,H14H,H14I), C150(H15A,H15B,H15C), C151(H15D,H15E,H15F),
 C154(H15K,H15L,H15M), C155(H15N,H15O,H15P), C158(H15U,H15V,H15W), C159(H15X,
 H15Y,H), C162(H16E,H16F,H16G), C93(H93A,H93B,H93C), C96(H96A,H96B,H96C),
 C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C102(H10E,H10F,H10G), C103(H10H,H10I,
 H10J), C104(H10K,H10L,H10M), C107(H10R,H10S,H10T), C201(H20F,H20G,H20H),
 C204(H20M,H20N,H20O), C205(H20P,H20Q,H20R), C208(H20W,H20X,H20Y), C209(H20Z,HA,
 HB), C212(H21H,H21I,H21J), C213(H21K,H21L,H21M), C216(H21R,H21S,H21T),
 C1B(H1BA,H1BB,H1BC)
;
_shelx_res_checksum              70283
_olex2_submission_special_instructions 'No special instructions were received'