Cobalt PCP Pincer Complexes via an Unexpected Sequence of Ortho Metalations
Kent, Mark A.; Woodall, Christopher H.; Haddow, Mairi F.; McMullin, Claire L.; Pringle, Paul G.; Wass, Duncan F.; Organometallics 33 (2014) 5686–; doi:10.1021/om500079j

data_4083053
_publ_section_title
;
 Cobalt PCP Pincer Complexes via an Unexpected Sequence of Ortho
 Metalations
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5686
_journal_paper_doi               10.1021/om500079j
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C38 H45 Co P4'
_chemical_formula_sum            'C38 H45 Co P4'
_chemical_formula_weight         684.55
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.708(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.7907(3)
_cell_length_b                   20.2094(8)
_cell_length_c                   35.0149(8)
_cell_measurement_temperature    100.0
_cell_volume                     6925.1(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.813
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            69848
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.370
_diffrn_reflns_theta_min         1.539
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.60534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.781
_refine_diff_density_min         -1.250
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1549
_refine_ls_number_reflns         34396
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0961
_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^)+(0.0560P)^2^+81.9819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.2410
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.813
_reflns_number_gt                26230
_reflns_number_total             34396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500079j_si_001.cif
_cod_data_source_block           shelxs
_cod_database_code               4083053
_shelxl_version_number           2013-3
_olex2_refinement_description
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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. Uiso/Uaniso restraints and constraints
: with sigma of 0.05 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.05 and sigma for terminal atoms of 0.2
: with sigma of 0.05 and sigma for terminal atoms of 0.1
: with sigma of 0.05 and sigma for terminal atoms of 0.1
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C53(H53A,H53B), C60(H60A,H60B), C99(H99A,
 H99B), C118(H11S,H11T), C133(H13C,H13D), C140(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C42(H42),
 C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51),
  C52(H52), C55(H55), C56(H56), C57(H57), C62(H62), C63(H63), C64(H64),
 C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C82(H82),
  C83(H83), C84(H84), C85(H85), C86(H86), C88(H88), C89(H89), C90(H90),
 C91(H91), C92(H92), C94(H94), C95(H95), C96(H96), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C107(H107), C108(H108), C109(H109),
 C110(H110), C111(H111), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C135(H135), C136(H136), C137(H137), C142(H142), C143(H143), C144(H144),
 C145(H145), C146(H146), C148(H148), C149(H149), C150(H150), C151(H151),
 C152(H152)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C73(H73A,H73B,H73C), C74(H74A,
 H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C),
 C78(H78A,H78B,H78C), C112(H11A,H11B,H11C), C113(H11D,H11E,H11F), C114(H11G,
 H11H,H11I), C115(H11J,H11K,H11L), C116(H11M,H11N,H11O), C117(H11P,H11Q,H11R),
 C177(H17A,H17B,H17C), C178(H17D,H17E,H17F), C179(H17G,H17H,H17I), C180(H18A,
 H18B,H18C), C181(H18D,H18E,H18F), C182(H18G,H18H,H18I)
;