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_4085119
_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         'C29 H21, 2(C10 H20 K0.5 O4), C4 H8 O'
_chemical_formula_sum            'C53 H69 K O9'
_chemical_formula_weight         889.18
_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                78.32(3)
_cell_angle_beta                 89.11(3)
_cell_angle_gamma                73.78(3)
_cell_formula_units_Z            2
_cell_length_a                   10.123(2)
_cell_length_b                   12.975(3)
_cell_length_c                   19.538(4)
_cell_measurement_reflns_used    14279
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.160
_cell_measurement_theta_min      1.065
_cell_volume                     2410.8(10)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.776
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Silicon Double Crystal'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.920
_diffrn_reflns_Laue_measured_fraction_max 0.776
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33659
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.776
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.160
_diffrn_reflns_theta_min         1.065
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.9983
_exptl_absorpt_correction_T_min  0.9918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       plate
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         14279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.6021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9956
_reflns_number_total             14279
_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_original_cell_volume        2410.8(9)
_cod_database_code               4085119
_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
2. Others
 Fixed Sof: H46C(0.5) H46D(0.5) H46A(0.5) H46B(0.5) H48C(0.5) H48D(0.5)
 H48A(0.5) H48B(0.5) C47A(0.5) H47A(0.5) H47B(0.5) C47B(0.5) H47C(0.5)
 H47D(0.5) H37A(0.5) H37B(0.5) H37C(0.5) H37D(0.5) C36(0.5) H36A(0.5) H36B(0.5)
 C36A(0.5) H36C(0.5) H36D(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46C,H46D), C46(H46A,H46B), C48(H48C,H48D),
 C48(H48A,H48B), C49(H49A,H49B), C47A(H47A,H47B), C47B(H47C,H47D), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C37(H37A,H37B), C37(H37C,H37D), C38(H38A,H38B), C39(H39A,H39B),
  C36(H36A,H36B), C36A(H36C,H36D), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,
 H52B), C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
;
_shelx_res_checksum              26831
_shelx_hkl_checksum              87235
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'