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_4085114
_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         'C58 H42 Mg'
_chemical_formula_sum            'C58 H42 Mg'
_chemical_formula_weight         763.22
_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                66.47(3)
_cell_angle_beta                 76.50(3)
_cell_angle_gamma                87.23(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2040(16)
_cell_length_b                   10.755(2)
_cell_length_c                   12.969(3)
_cell_measurement_reflns_used    34097
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.797
_cell_measurement_theta_min      1.761
_cell_volume                     1018.9(5)
_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    'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Silicon Double Crystal'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34097
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.796
_diffrn_reflns_theta_min         1.761
_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    0.084
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.9992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       block
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1042P)^2^+0.4607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3940
_reflns_number_total             5085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501150b_si_001.cif
_cod_data_source_block           merge
_cod_depositor_comments
'Adding full bibliography for 4085114--4085119.cif.'
_cod_original_cell_volume        1018.9(4)
_cod_database_code               4085114
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.032) H7(0.036) H8(0.039) H9(0.041) H10(0.041) H11(0.036)
 H13(0.037) H14(0.041) H15(0.044) H16(0.04) H17(0.036) H19(0.039) H20(0.049)
 H21(0.054) H22(0.05) H23(0.04) H25(0.035) H26(0.041) H27(0.043) H28(0.04)
 H29(0.035)
 Fixed X: Mg1(1) H1(0.7455) H7(0.8641) H8(0.8922) H9(0.8012) H10(0.6784)
 H11(0.657) H13(0.9699) H14(0.9467) H15(0.7108) H16(0.4987) H17(0.5239)
 H19(0.9313) H20(0.924) H21(0.7293) H22(0.5323) H23(0.5381) H25(0.8555)
 H26(0.8533) H27(0.7269) H28(0.6066) H29(0.6123)
 Fixed Y: Mg1(0) H1(-0.1903) H7(-0.1556) H8(-0.1398) H9(0.0499) H10(0.2227)
 H11(0.2113) H13(0.3097) H14(0.5414) H15(0.6507) H16(0.5279) H17(0.2968)
 H19(0.294) H20(0.4229) H21(0.3645) H22(0.1843) H23(0.0552) H25(-0.0616) H26(-
 0.2311) H27(-0.4461) H28(-0.4901) H29(-0.3232)
 Fixed Z: Mg1(0.5) H1(0.5254) H7(0.3293) H8(0.1418) H9(0.0042) H10(0.0579)
 H11(0.2436) H13(0.2703) H14(0.1672) H15(0.2234) H16(0.3859) H17(0.4904)
 H19(0.5394) H20(0.6489) H21(0.8254) H22(0.8887) H23(0.7796) H25(0.7972)
 H26(0.979) H27(1.0346) H28(0.9052) H29(0.7227)
;
_shelx_res_checksum              67302
_shelx_hkl_checksum              93369
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'