Alkali metal and stoichiometric effects in intermolecular hydroamination catalysed by lithium, sodium and potassium magnesiates.
Davin, Laia; Hernán-Gómez, Alberto; McLaughlin, Calum; Kennedy, Alan R.; McLellan, Ross; Hevia, Eva; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8122–8130; doi:10.1039/c9dt00923j

data_7049722
_publ_section_title
;
 Alkali metal and stoichiometric effects in intermolecular hydroamination
 catalysed by lithium, sodium and potassium magnesiates.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8122
_journal_page_last               8130
_journal_paper_doi               10.1039/c9dt00923j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H72 Mg N8 Na2'
_chemical_formula_sum            'C32 H72 Mg N8 Na2'
_chemical_formula_weight         639.26
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-01 deposited with the CCDC.    2019-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.733(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4760(14)
_cell_length_b                   19.224(2)
_cell_length_c                   19.864(2)
_cell_measurement_reflns_used    5093
_cell_measurement_temperature    123.6
_cell_measurement_theta_max      27.9319
_cell_measurement_theta_min      3.0931
_cell_volume                     3991.9(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.6
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -16.00  109.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9130   77.0000   90.0000 125

  2 omega    3.00   96.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9130   77.0000  150.0000 93

  3 omega  -83.00  -36.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.6942  179.0000 -120.0000 47

  4 omega  -71.00   26.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.6942   37.0000 -180.0000 97
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0563729000
_diffrn_orient_matrix_UB_12      -0.0203556000
_diffrn_orient_matrix_UB_13      -0.0006998000
_diffrn_orient_matrix_UB_21      -0.0076182000
_diffrn_orient_matrix_UB_22      -0.0012554000
_diffrn_orient_matrix_UB_23      -0.0357049000
_diffrn_orient_matrix_UB_31      0.0370486000
_diffrn_orient_matrix_UB_32      0.0307518000
_diffrn_orient_matrix_UB_33      -0.0019468000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0953
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19600
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.099
_diffrn_source                   'Oxford Diffraction Xcalibur E'
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7810
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0979P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.2205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4183
_reflns_number_total             7810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00923j2.cif
_cod_data_source_block           ahg26xsmart2
_cod_depositor_comments
'Adding full bibliography for 7049721--7049722.cif.'
_cod_database_code               7049722
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-C21 = C22A-C21A
 1.53 with sigma of 0.01
 N6-C22 = N6-C25 = N6-C26 = N5-C21 = N5-C23 = N5-C24
 1.48 with sigma of 0.01
 N6A-C22A = N6A-C25A = N6A-C26A = N5-C21A = N5-C23A = N5-C24A
 1.48 with sigma of 0.01
3. Rigid bond restraints
 N5, N6, C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N5 \\sim N6 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(N6) = Uanis(N6A)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
Uanis(C22) = Uanis(C22A)
Uanis(C21) = Uanis(C21A)
5. Others
 Sof(N6A)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(N6)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
  C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C27(H27A,H27B), C28(H28A,
 H28B), C21A(H21C,H21D), C22A(H22C,H22D)
6.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C24A(H24D,H24E,H24F), C23A(H23D,H23E,H23F), C25A(H25D,H25E,H25F),
 C26A(H26D,H26E,H26F)
;
_shelx_res_checksum              55273
_olex2_submission_special_instructions 'No special instructions were received'