Acyclic 1,2-Dimagnesioethanes/-ethene Derived from Magnesium(I) Compounds: Multipurpose Reagents for Organometallic Synthesis
Jones, Cameron; Dange, Deepak; Gair, Andrew; Jones, Dafydd; Juckel, Martin; Aldridge, Simon; Chemical Science  (2019) –; doi:10.1039/C9SC00200F

data_1550546
_publ_section_title
;
 Acyclic 1,2-Dimagnesioethanes/-ethene Derived from Magnesium(I)
 Compounds: Multipurpose Reagents for Organometallic Synthesis
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00200F
_journal_year                    2019
_chemical_formula_sum            'C93 H114 B2 Cd2 N6 Si2'
_chemical_formula_weight         1618.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-01-11 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.733(3)
_cell_length_b                   27.815(6)
_cell_length_c                   11.021(2)
_cell_measurement_reflns_used    7903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.93
_cell_volume                     4516.4(16)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29143
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.248
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         2.930
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.9378
_exptl_absorpt_correction_T_min  0.9010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.969
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 3178 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7903
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0645P)^2^+4.9816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                7536
_reflns_number_total             7903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00200f2.cif
_cod_data_source_block           Cj1322
_cod_database_code               1550546
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              15580