Alkaline Earth-centered CO Homologation, Reduction and Amine Carbonylation.
Anker, Mathew D.; Kefalidis, Christos E.; Yang, Yan; Fang, Jian; Hill, Michael S.; Mahon, Mary F.; Maron, Laurent; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b04926

data_4126276
_publ_section_title
;
 Alkaline Earth-centered CO Homologation, Reduction and Amine
 Carbonylation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b04926
_journal_year                    2017
_chemical_formula_moiety         'C37 H49 Mg N3 O, C3 H3'
_chemical_formula_sum            'C40 H52 Mg N3 O'
_chemical_formula_weight         615.15
_chemical_name_systematic
;
 ?
;
_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   geom
_audit_creation_date             2017-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.0066(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.88039(16)
_cell_length_b                   11.90132(12)
_cell_length_c                   21.6100(2)
_cell_measurement_reflns_used    11860
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.6990
_cell_measurement_theta_min      3.5150
_cell_volume                     3515.56(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22341
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.757
_diffrn_reflns_theta_min         3.526
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.248
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0688P)^2^+2.4594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5938
_reflns_number_total             6584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04926_si_002.cif
_cod_data_source_block           s16msh1-cpd-26
_cod_original_cell_volume        3515.56(7)
_cod_database_code               4126276
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C12(H12), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C22(H22), C20(H20), C21(H21), C37(H37), C36(H36), C33(H33), C8(H8),
 C9(H9), C10(H10), C35(H35), C34(H34), C39(H39), C40(H40), C38(H38)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C),
 C29(H29A,H29B,H29C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C31(H31A,H31B,
 H31C), C26(H26A,H26B,H26C), C16(H16A,H16B,H16C), C28(H28A,H28B,H28C)
;