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_4085116
_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 Ca2 O4, 3(C4 H8 O)'
_chemical_formula_sum            'C86 H98 Br2 Ca2 O7'
_chemical_formula_weight         1483.62
_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             2014-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                92.999(3)
_cell_angle_beta                 90.558(2)
_cell_angle_gamma                115.076(2)
_cell_formula_units_Z            1
_cell_length_a                   11.3598(6)
_cell_length_b                   12.5296(9)
_cell_length_c                   14.3526(7)
_cell_measurement_reflns_used    8636
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      28.321
_cell_measurement_theta_min      2.456
_cell_volume                     1846.63(19)
_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      123.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20718
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.497
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         3.420
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0776 before and 0.0358 after correction.
The Ratio of minimum to maximum transmission is 0.9576.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8439
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0396P)^2^+1.2032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7003
_reflns_number_total             8439
_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               4085116
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.782
_olex2_refinement_description
;
1. Others
 Fixed Sof: C44(0.5) H44A(0.5) H44B(0.5) C43(0.5) H43A(0.5) H43B(0.5) C42(0.5)
 H42A(0.5) H42B(0.5) C45(0.5) H45A(0.5) H45B(0.5) O4(0.5)
 Fixed Uiso: H1(0.015) H19(0.019) H17(0.023) H13(0.022) H11(0.022) H10(0.031)
 H29(0.023) H23(0.021) H25(0.023) H16(0.027) H8(0.029) H20(0.025) H15(0.025)
 H14(0.028) H7(0.021) H21(0.027) H34A(0.03) H34B(0.03) H33A(0.029) H33B(0.029)
 H37A(0.031) H37B(0.031) H22(0.026) H36A(0.034) H36B(0.034) H30A(0.032)
 H30B(0.032) H26(0.032) H27(0.034) H35A(0.04) H35B(0.04) H9(0.034) H28(0.032)
 H31A(0.046) H31B(0.046) H32A(0.045) H32B(0.045) H38A(0.046) H38B(0.046)
 H39A(0.045) H39B(0.045) H41A(0.055) H41B(0.055) H40A(0.066) H40B(0.066)
 H44A(0.046) H44B(0.046) H43A(0.045) H43B(0.045) H42A(0.045) H42B(0.045)
 H45A(0.041) H45B(0.041)
 Fixed X: H1(0.5506) H19(0.4792) H17(0.7772) H13(0.7131) H11(0.8485)
 H10(1.0428) H29(0.3715) H23(0.3932) H25(0.2272) H16(0.9249) H8(0.9841)
 H20(0.3865) H15(0.9724) H14(0.8626) H7(0.79) H21(0.2985) H34A(0.1642)
 H34B(0.1385) H33A(0.5907) H33B(0.4508) H37A(0.3477) H37B(0.3211) H22(0.3031)
 H36A(0.128) H36B(0.1311) H30A(0.5826) H30B(0.7107) H26(0.0209) H27(-0.0122)
 H35A(0.0747) H35B(-0.0067) H9(1.1108) H28(0.163) H31A(0.7816) H31B(0.711)
 H32A(0.527) H32B(0.6354) H38A(0.3591) H38B(0.2136) H39A(0.2209) H39B(0.377)
 H41A(0.3021) H41B(0.4394) H40A(0.3251) H40B(0.1899) H44A(0.1095) H44B(0.0592)
 H43A(-0.1442) H43B(-0.0966) H42A(-0.1421) H42B(-0.1345) H45A(0.2035)
 H45B(0.0977)
 Fixed Y: H1(0.9545) H19(0.7102) H17(0.9542) H13(0.6829) H11(1.1065)
 H10(1.264) H29(0.7939) H23(0.5538) H25(0.6793) H16(0.9067) H8(1.1565)
 H20(0.5254) H15(0.752) H14(0.6374) H7(0.9997) H21(0.3547) H34A(0.9633)
 H34B(0.8415) H33A(1.287) H33B(1.239) H37A(1.0007) H37B(1.108) H22(0.3695)
 H36A(1.0049) H36B(0.8793) H30A(1.1895) H30B(1.1894) H26(0.5803) H27(0.5887)
 H35A(1.025) H35B(0.8848) H9(1.2902) H28(0.6977) H31A(1.3788) H31B(1.3858)
 H32A(1.3682) H32B(1.4441) H38A(0.5216) H38B(0.4231) H39A(0.3938) H39B(0.4417)
 H41A(0.2003) H41B(0.2842) H40A(0.2479) H40B(0.214) H44A(0.5039) H44B(0.6061)
 H43A(0.4778) H43B(0.3735) H42A(0.4809) H42B(0.3559) H45A(0.6041) H45B(0.6568)
 Fixed Z: H1(0.1285) H19(0.4616) H17(0.464) H13(0.276) H11(0.3539) H10(0.3208)
 H29(0.0309) H23(0.2007) H25(0.2816) H16(0.5463) H8(0.0473) H20(0.523)
 H15(0.4912) H14(0.3573) H7(0.0797) H21(0.4238) H34A(0.3781) H34B(0.3203)
 H33A(0.3871) H33B(0.3339) H37A(0.1451) H37B(0.1912) H22(0.2627) H36A(0.1115)
 H36B(0.1267) H30A(0.1382) H30B(0.187) H26(0.2126) H27(0.0526) H35A(0.2636)
 H35B(0.2415) H9(0.1669) H28(-0.0372) H31A(0.2452) H31B(0.1491) H32A(0.2218)
 H32B(0.3016) H38A(0.0243) H38B(0.0362) H39A(-0.118) H39B(-0.115) H41A(0.0458)
 H41B(0.0045) H40A(-0.129) H40B(-0.0771) H44A(0.4121) H44B(0.4073) H43A(0.432)
 H43B(0.424) H42A(0.5863) H42B(0.575) H45A(0.548) H45B(0.561)
;
_shelx_res_checksum              19742
_shelx_hkl_checksum              59036
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'