π Ligands in Alkaline Earth Complexes
Roşca, Sorin-Claudiu; Caytan, Elsa; Dorcet, Vincent; Roisnel, Thierry; Carpentier, Jean-François; Sarazin, Yann; Organometallics 36 (2017) 1269–; doi:10.1021/acs.organomet.7b00006

data_4089218
_publ_section_title
;
 \p Ligands in Alkaline Earth Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1269
_journal_paper_doi               10.1021/acs.organomet.7b00006
_journal_volume                  36
_journal_year                    2017
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C42 H84 Ca3 F12 N6 O2 Si8'
_chemical_formula_sum            'C42 H84 Ca3 F12 N6 O2 Si8'
_chemical_formula_weight         1278.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.203(3)
_cell_angle_beta                 92.382(2)
_cell_angle_gamma                91.935(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3294(7)
_cell_length_b                   16.6381(12)
_cell_length_c                   18.2154(13)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.33
_cell_measurement_wavelength     0.71073
_cell_volume                     3307.0(4)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
          WinGX publication routines (Farrugia, 2012),
          CRYSCALc (T. Roisnel, local program, 2014)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46479
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.590
_exptl_crystal_size_min          0.370
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         14810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+1.4698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                11823
_reflns_number_total             14810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00006_si_002.cif
_cod_data_source_block           '[5-Ca)]3'
_cod_database_code               4089218