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_7049721
_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         'C46 H92 Mg2 N6 Na2 O4, 2(C4 H8 O)'
_chemical_formula_sum            'C54 H108 Mg2 N6 Na2 O6'
_chemical_formula_weight         1032.06
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-02-28
_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                100.805(4)
_cell_angle_beta                 94.008(3)
_cell_angle_gamma                106.319(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6474(5)
_cell_length_b                   11.7398(7)
_cell_length_c                   23.4025(8)
_cell_measurement_reflns_used    13875
_cell_measurement_temperature    123.0
_cell_measurement_theta_max      73.1413
_cell_measurement_theta_min      3.8761
_cell_measurement_wavelength     1.5418
_cell_volume                     2991.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.0
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega -106.00  -53.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  120.0000 53

  2 omega -112.00  -21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -50.0000    0.0000 91

  3 omega  -41.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  120.0000 29

  4 omega  -95.00  -11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  125.0000  120.0000 84

  5 omega  -13.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -77.0000    0.0000 32

  6 omega   39.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -132.0000   -6.0000 49

  7 omega  -16.00   25.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -37.0000  -90.0000 41

  8 omega   34.00  124.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   65.0000 -141.0000 90

  9 omega   20.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -77.0000    0.0000 58

 10 omega  -12.00   15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -37.0000 -120.0000 27

 11 omega   24.00   50.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   80.0000 -111.0000 26

 12 omega   29.00  124.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   71.0000  120.0000 95

 13 omega   78.00  150.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  179.0000  -30.0000 72

 14 omega   63.00  144.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  179.0000  -90.0000 81

 15 omega   41.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -115.0000   24.0000 64

 16 omega   98.00  145.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   30.0000 47

 17 omega   90.00  135.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000   30.0000 45

 18 omega   88.00  132.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -30.0000 44

 19 omega   94.00  125.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000   30.0000 31

 20 omega   82.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -120.0000 57

 21 omega   93.00  119.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -60.0000 26

 22 omega   87.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -180.0000 26

 23 omega   57.00  131.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  179.0000  -60.0000 74

 24 omega   89.00  128.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -150.0000 39

 25 omega   51.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -136.0000   -4.0000 76

 26 omega   81.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  -30.0000 45

 27 omega   90.00  172.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  132.0000 -117.0000 82

 28 omega   64.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -113.0000   46.0000 27

 29 omega   88.00  144.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -180.0000 56

 30 omega   58.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  179.0000    0.0000 81

 31 omega   88.00  125.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -90.0000 37

 32 omega   41.00  119.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -120.0000  105.0000 78

 33 omega -113.00  -11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -79.0000 -141.0000 102

 34 omega  -16.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -37.0000   60.0000 44

 35 omega  -16.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -37.0000 -150.0000 44

 36 omega  -16.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -37.0000  -60.0000 44

 37 omega   24.00   50.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   80.0000  161.0000 26

 38 omega   25.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   79.0000  -12.0000 102

 39 omega   28.00  125.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   73.0000   80.0000 97

 40 omega   29.00  125.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   71.0000  -72.0000 96

 41 omega  -16.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -37.0000    0.0000 44

 42 omega   90.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000   30.0000 88

 43 omega   90.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000 -180.0000 88

 44 omega   78.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000    0.0000 100

 45 omega   78.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000  120.0000 100

 46 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -90.0000 96

 47 omega   78.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000  -90.0000 100

 48 omega   90.00  140.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000 -150.0000 50

 49 omega   40.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -115.0000   76.0000 77

 50 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  120.0000 96
;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0806498000
_diffrn_orient_matrix_UB_12      -0.0367070000
_diffrn_orient_matrix_UB_13      -0.0595263000
_diffrn_orient_matrix_UB_21      -0.1113912000
_diffrn_orient_matrix_UB_22      -0.0014841000
_diffrn_orient_matrix_UB_23      0.0320274000
_diffrn_orient_matrix_UB_31      0.0201662000
_diffrn_orient_matrix_UB_32      0.1351658000
_diffrn_orient_matrix_UB_33      -0.0006670000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         73.290
_diffrn_reflns_theta_min         5.824
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
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    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         11830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0996P)^2^+0.9844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9231
_reflns_number_total             11830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00923j2.cif
_cod_data_source_block           calum1b
_cod_depositor_comments
'Adding full bibliography for 7049721--7049722.cif.'
_cod_database_code               7049721
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B)
;
_shelx_res_checksum              50877
_olex2_submission_special_instructions 'No special instructions were received'