A Scandium Complex Bearing Both Methylidene and Phosphinidene Ligands: Synthesis, Structure, and Reactivity
Zhou, Jiliang; Li, Tengfei; Maron, Laurent; Leng, Xuebing; Chen, Yaofeng; Organometallics 34 (2015) 470–; doi:10.1021/om500997j

data_4085175
_publ_section_title
;
 A Scandium Complex Bearing Both Methylidene and Phosphinidene Ligands:
 Synthesis, Structure, and Reactivity
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              470
_journal_paper_doi               10.1021/om500997j
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C71 H101 N4 P Sc2, C3 H7'
_chemical_formula_sum            'C74 H108 N4 P Sc2'
_chemical_formula_weight         1174.53
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.889(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.123(3)
_cell_length_b                   13.2323(13)
_cell_length_c                   24.521(2)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.494
_cell_measurement_theta_min      2.18
_cell_volume                     7333.6(13)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      140.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51453
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.664
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0787 before and 0.0609 after correction.
The Ratio of minimum to maximum transmission is 0.8617.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       plate
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         2.696
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         14370
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+4.6413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10398
_reflns_number_total             14370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500997j_si_002.cif
_cod_data_source_block           dm13434
_cod_depositor_comments
'Adding full bibliography for 4085175--4085180.cif.'
_cod_original_cell_volume        7333.5(12)
_cod_database_code               4085175
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.932
_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. Restrained distances
 Sc1-C71 \\sim Sc2-C71
 with sigma of 0.01
3. Rigid bond restraints
 Sc2, C71
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C46 \\sim C44: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
C56 \\sim C57 \\sim C58: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C46) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C71) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C41(H41), C44(H44), C53(H53),
 C56(H56), C65(H65), C68(H68)
5.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C37(H37), C38(H38), C39(H39), C49(H49), C50(H50), C51(H51), C61(H61), C62(H62),
  C63(H63)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,
 H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,
 H69B,H69C), C70(H70A,H70B,H70C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              87619
_shelx_hkl_checksum              60393
_olex2_submission_special_instructions 'No special instructions were received'