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_4085118
_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 H74 Br2 O4 Yb2, 4(C7 H8)'
_chemical_formula_sum            'C102 H106 Br2 O4 Yb2'
_chemical_formula_weight         1901.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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             2014-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                66.7020(10)
_cell_angle_beta                 81.237(2)
_cell_angle_gamma                83.161(2)
_cell_formula_units_Z            1
_cell_length_a                   11.8774(4)
_cell_length_b                   12.5527(4)
_cell_length_c                   15.7359(5)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.375
_cell_measurement_theta_min      2.368
_cell_volume                     2125.19(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 0.992
_diffrn_measured_fraction_theta_max 0.986
_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  0.0212
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35431
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.400
_diffrn_reflns_theta_min         3.478
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.179
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0662 before and 0.0318 after correction.
The Ratio of minimum to maximum transmission is 0.8038.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         10513
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+1.6610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9658
_reflns_number_total             10513
_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               4085118
_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. Uiso/Uaniso restraints and constraints
Uanis(C51) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq:
with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C33(H33A,H33B), C37(H37A,H37B), C32(H32A,H32B), C35(H35A,
 H35B), C34(H34A,H34B), C31(H31A,H31B), C36(H36A,H36B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C11(H11), C28(H28), C22(H22), C7(H7), C25(H25), C19(H19), C13(H13),
 C17(H17), C21(H21), C26(H26), C23(H23), C29(H29), C10(H10), C20(H20), C27(H27),
  C8(H8), C15(H15), C9(H9), C40(H40), C39(H39), C43(H43), C16(H16), C42(H42),
 C14(H14), C41(H41), C50(H50), C49(H49), C46(H46), C47(H47), C48(H48)
3.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              17450
_shelx_hkl_checksum              14541
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'