A versatile nitrogen ligand for alkaline-earth chemistry.
Chapple, Peter M.; Cordier, Marie; Dorcet, Vincent; Roisnel, Thierry; Carpentier, Jean-François; Sarazin, Yann; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11878–11889; doi:10.1039/d0dt02236e

data_7704966
_publ_section_title
;
 A versatile nitrogen ligand for alkaline-earth chemistry.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11878
_journal_page_last               11889
_journal_paper_doi               10.1039/d0dt02236e
_journal_volume                  49
_journal_year                    2020
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C57 H85 Ba N3 O Si2'
_chemical_formula_sum            'C57 H85 Ba N3 O Si2'
_chemical_formula_weight         1021.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-05-05 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.726(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0352(6)
_cell_length_b                   23.0649(12)
_cell_length_c                   19.3728(12)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5140
_cell_measurement_theta_min      2.1554
_cell_measurement_wavelength     0.71073
_cell_volume                     5681.5(5)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2016)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    "'SHELXT 2018_2 (Sheldrick, 2018)'"
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0042909
_diffrn_orient_matrix_UB_12      0.0171595
_diffrn_orient_matrix_UB_13      -0.0479560
_diffrn_orient_matrix_UB_21      0.0220459
_diffrn_orient_matrix_UB_22      0.0384672
_diffrn_orient_matrix_UB_23      0.0221793
_diffrn_orient_matrix_UB_31      0.0753724
_diffrn_orient_matrix_UB_32      -0.0102745
_diffrn_orient_matrix_UB_33      0.0029464
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51447
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.533
_diffrn_reflns_theta_min         2.155
_diffrn_source_current           1.0
_diffrn_source_voltage           55.0
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       plate
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.149
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         12975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+17.1680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10930
_reflns_number_total             12975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt02236e2.cif
_cod_data_source_block           PC084
_cod_depositor_comments
'Adding full bibliography for 7704966--7704975.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7704966
_shelx_res_checksum              84190