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_7704971
_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         'C62.15 H100 Ca N3 O1.35 Si3 Sn'
_chemical_formula_sum            'C62.15 H100 Ca N3 O1.35 Si3 Sn'
_chemical_formula_weight         1153.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-07-29 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.784(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0735(18)
_cell_length_b                   20.434(2)
_cell_length_c                   25.973(3)
_cell_measurement_reflns_used    9573
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5369
_cell_measurement_theta_min      2.4571
_cell_measurement_wavelength     0.71073
_cell_volume                     6935.2(14)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'PLATON, A.L.Spek, Acta Cryst. 2009, D65, 148-155'
_computing_publication_material
'CRYSCALC (T. Roisnel, local program, ver. 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (G. Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      0.0699404
_diffrn_orient_matrix_UB_12      0.0041655
_diffrn_orient_matrix_UB_13      0.0163759
_diffrn_orient_matrix_UB_21      0.0251818
_diffrn_orient_matrix_UB_22      -0.0356177
_diffrn_orient_matrix_UB_23      -0.0227708
_diffrn_orient_matrix_UB_31      0.0181858
_diffrn_orient_matrix_UB_32      0.0332999
_diffrn_orient_matrix_UB_33      -0.0264042
_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  0.0860
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            50853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.952
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       prism
_exptl_crystal_F_000             2467
_exptl_crystal_size_max          0.680
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.240
_refine_diff_density_max         1.748
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         15634
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0638P)^2^+9.5031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11028
_reflns_number_total             15634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt02236e2.cif
_cod_data_source_block           PC469_2
_cod_depositor_comments
'Adding full bibliography for 7704966--7704975.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7704971
_shelx_res_checksum              59380
_shelx_fab_checksum              1250