Hydroamination of isocyanates and isothiocyanates by alkaline earth metal initiators supported by a bulky iminopyrrolyl ligand
Bano, Kulsum; Anga, Srinivas; Jain, Archana; Nayek, Hari Pada; Panda, Tarun K.; New Journal of Chemistry 44 (2020) 9419–9428; doi:10.1039/D0NJ01509A

data_7059589
_publ_section_title
;
 Hydroamination of isocyanates and isothiocyanates by alkaline earth metal
 initiators supported by a bulky iminopyrrolyl ligand
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9419
_journal_page_last               9428
_journal_paper_doi               10.1039/D0NJ01509A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C64 H52 Ba N6'
_chemical_formula_sum            'C64 H52 Ba N6'
_chemical_formula_weight         1042.493
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2020-04-21
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.03.26 svn.re84ffbc8 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-05-03 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.423(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0821(2)
_cell_length_b                   26.7914(7)
_cell_length_c                   19.1056(4)
_cell_measurement_reflns_used    9011
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.2470
_cell_measurement_theta_min      3.2740
_cell_volume                     5039.6(2)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_collection
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9826
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.9826
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19646
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9826
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         71.28
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    6.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64681
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             2140.374
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.9313
_refine_diff_density_min         -1.1619
_refine_diff_density_rms         0.0753
_refine_ls_d_res_high            0.8140
_refine_ls_d_res_low             13.4612
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0571
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    129
_refine_ls_number_parameters     777
_refine_ls_number_reflns         9611
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.0565
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.8370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -14
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                8371
_reflns_number_total             9611
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0nj01509a2.cif
_cod_data_source_block           6
_cod_depositor_comments
;Adding full bibliography for 7059585--7059589.cif.

 Adding full bibliography for 7059585--7059589.cif.
;
_cod_database_code               7059589
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Ba1-N5 \\sim Ba1-N5A
 with sigma of 0.02
3. Rigid bond restraints
 C37B, N5A, N5, C37A, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(N5A)=1-FVAR(1)
 Sof(N5)=FVAR(1)
 Fixed Sof: C37B(0.5) H37B(0.5) C39A(0.5) H39A(0.5) C40(0.5) C41(0.5) H41(0.5)
 C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5) H45(0.5)
 C47(0.5) C46(0.5) H46(0.5) C51(0.5) H51(0.5) C50(0.5) H50(0.5) C49(0.5)
 H49(0.5) C48(0.5) H48(0.5) C39B(0.5) H39B(0.5) C40A(0.5) C41A(0.5) H41A(0.5)
 C42A(0.5) H42A(0.5) C43A(0.5) H43A(0.5) C44A(0.5) H44A(0.5) C45A(0.5)
 H45A(0.5) C46A(0.5) H46A(0.5) C47A(0.5) C48A(0.5) H48A(0.5) C49A(0.5)
 H49A(0.5) C50A(0.5) H50A(0.5) C51A(0.5) H51A(0.5) C37A(0.5) H37A(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C20(H20), C39A(H39A), C52(H52), C39B(H39B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C37B(H37B), C38(H38), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45), C46(H46), C51(H51), C50(H50), C49(H49), C48(H48),
  C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
 C62(H62), C63(H63), C64(H64), C41A(H41A), C42A(H42A), C43A(H43A), C44A(H44A),
 C45A(H45A), C46A(H46A), C48A(H48A), C49A(H49A), C50A(H50A), C51A(H51A),
 C37A(H37A)
;
_olex2_submission_special_instructions 'No special instructions were received'