Bulky Group 2 Octaphenylmetallocenes and Direct Access to Calcium and Ytterbium Pseudo-Grignard Complexes
Deacon, Glen B.; Jaroschik, Florian; Junk, Peter C.; Kelly, Rory P.; Organometallics 34 (2015) 2369–; doi:10.1021/om501150b

data_4085117
_publ_section_title
;
 Bulky Group 2 Octaphenylmetallocenes and Direct Access to Calcium and
 Ytterbium Pseudo-Grignard Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2369
_journal_paper_doi               10.1021/om501150b
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C74 H58 Br2 O4 Yb2, 3(C4 H8 O)'
_chemical_formula_sum            'C86 H82 Br2 O7 Yb2'
_chemical_formula_weight         1733.41
_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
_audit_creation_date             2014-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                93.069(2)
_cell_angle_beta                 90.738(2)
_cell_angle_gamma                115.190(2)
_cell_formula_units_Z            1
_cell_length_a                   11.3758(4)
_cell_length_b                   12.5225(5)
_cell_length_c                   14.3701(5)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      2.39
_cell_volume                     1848.30(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.964
_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  0.0205
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21750
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.568
_diffrn_reflns_theta_min         3.264
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.650
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1130 before and 0.0309 after correction.
The Ratio of minimum to maximum transmission is 0.8851.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9095
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+1.4632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8228
_reflns_number_total             9095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501150b_si_001.cif
_cod_data_source_block           tri
_cod_depositor_comments
'Adding full bibliography for 4085114--4085119.cif.'
_cod_database_code               4085117
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O3-C100 \\sim O3-C103 \\sim O4-C104 \\sim O4-C107
 with sigma of 0.02
 C100-C101 \\sim C102-C103 \\sim C104-C105 \\sim C106-C107
 with sigma of 0.01
 C101-C102 \\sim C105-C106
 with sigma of 0.01
 O3-C101 \\sim O3-C102 \\sim O4-C105 \\sim O4-C106
 with sigma of 0.02
 C100-C102 \\sim C101-C103 \\sim C104-C106 \\sim C105-C107
 with sigma of 0.02
3. Others
 Fixed Sof: C104(0.5) H10I(0.5) H10J(0.5) C107(0.5) H10K(0.5) H10L(0.5)
 O4(0.5) C106(0.5) H10M(0.5) H10N(0.5) C105(0.5) H10O(0.5) H10P(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C34(H34A,H34B), C36(H36A,H36B), C35(H35A,H35B), C100(H10A,
 H10B), C102(H10C,H10D), C103(H10E,H10F), C101(H10G,H10H), C104(H10I,H10J),
 C107(H10K,H10L), C106(H10M,H10N), C105(H10O,H10P)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C19(H19), C14(H14), C20(H20), C29(H29), C17(H17), C25(H25), C11(H11),
 C22(H22), C7(H7), C21(H21), C10(H10), C16(H16), C13(H13), C23(H23), C15(H15),
 C8(H8), C27(H27), C26(H26), C9(H9), C28(H28)
;
_shelx_res_checksum              85627
_shelx_hkl_checksum              8108
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'