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_7704972
_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_absolute_configuration rm/ad/rmad/syn/unk/.
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C62 H78 Ca I N3 O'
_chemical_formula_sum            'C62 H78 Ca I N3 O'
_chemical_formula_weight         1048.25
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-05-15 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.1903(5)
_cell_length_b                   27.1903
_cell_length_c                   15.5907(7)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.4976
_cell_measurement_theta_min      2.5994
_cell_measurement_wavelength     0.71073
_cell_volume                     11526.4(6)
_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, 2019)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0225802
_diffrn_orient_matrix_UB_12      -0.0114599
_diffrn_orient_matrix_UB_13      -0.0465168
_diffrn_orient_matrix_UB_21      0.0222409
_diffrn_orient_matrix_UB_22      0.0148875
_diffrn_orient_matrix_UB_23      -0.0439931
_diffrn_orient_matrix_UB_31      0.0186570
_diffrn_orient_matrix_UB_32      -0.0316170
_diffrn_orient_matrix_UB_33      -0.0038545
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.001
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.728
_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    1.208
_exptl_crystal_description       stick
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.028(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         13207
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0397P)^2^+6.3586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                11796
_reflns_number_total             13207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt02236e2.cif
_cod_data_source_block           PC2099x2
_cod_depositor_comments
'Adding full bibliography for 7704966--7704975.cif.'
_cod_original_cell_volume        11526.4(7)
_cod_database_code               7704972
_shelx_res_checksum              26200