Cooperative dihydrogen activation at a Na(I)<sub>2</sub>/Mg(I)<sub>2</sub> ensemble.
Liu, Han-Ying; Neale, Samuel E.; Hill, Michael S.; Mahon, Mary F.; McMullin, Claire L.; Morrison, Benjamin L.; Chemical communications (Cambridge, England) 59 (2023) 3846–3849; doi:10.1039/d3cc00710c

data_7131355
_publ_section_title
;
 Cooperative dihydrogen activation at a
 Na(I)<sub>2</sub>/Mg(I)<sub>2</sub> ensemble.
;
_journal_issue                   26
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3846
_journal_page_last               3849
_journal_paper_doi               10.1039/d3cc00710c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C45 H76 Mg N3 Na2 Si3, C3 H7'
_chemical_formula_sum            'C48 H83 Mg N3 Na2 Si3'
_chemical_formula_weight         856.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-11-03 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                76.271(3)
_cell_angle_beta                 78.238(3)
_cell_angle_gamma                69.189(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4759(3)
_cell_length_b                   12.0459(4)
_cell_length_c                   23.1083(8)
_cell_measurement_reflns_used    13707
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.8250
_cell_measurement_theta_min      3.2280
_cell_volume                     2624.90(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45674
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.317
_diffrn_reflns_theta_min         2.961
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.084
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.391
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         13937
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0528P)^2^+0.8077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10400
_reflns_number_total             13937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00710c3.cif
_cod_data_source_block           e21msh26
_cod_depositor_comments          'Adding full bibliography for 7131355.cif.'
_cod_database_code               7131355
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Mg(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C48A
 1.54 with sigma of 0.02
 C46-C48 \\sim C46A-C48A
 with sigma of 0.02
 C47-C48 \\sim C47A-C48A
 with sigma of 0.02
 C46-C47 \\sim C46A-C47A
 with sigma of 0.04
 C48-C46A \\sim C48A-C46 \\sim C48-C47 \\sim C48A-C47A \\sim C47-C47_$1 \\sim
C47A-C47A_$1 ~
 C48_$1-C47_$1 \\sim C48A_$1-C47A_$1 \\sim C48A_$1-C46_$1 \\sim C48_$1-C46A_$1
 with sigma of 0.005
 C46A_$1-C47_$1 \\sim C48A_$1-C47A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C46A \\sim C46A \\sim C47 \\sim C47 \\sim C48 \\sim C48 \\sim C46 \\sim C46
\\sim C47A \\sim C47A \\sim C48A \\sim C48A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: C46A(0.7) H46A(0.7) H46B(0.7) H46C(0.7) C47(0.7) H47A(0.7)
 H47B(0.7) C48(0.7) H48A(0.7) H48B(0.7) C46(0.3) H46D(0.3) H46E(0.3) H46F(0.3)
 C47A(0.3) H47C(0.3) H47D(0.3) C48A(0.3) H48C(0.3) H48D(0.3)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C25(H25), C28(H28), C37(H37), C40(H40)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C45(H45A,H45B), C47(H47A,H47B), C48(H48A,
 H48B), C47A(H47C,H47D), C48A(H48C,H48D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C21(H21), C22(H22), C23(H23), C33(H33), C34(H34),
 C35(H35)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46A(H46A,H46B,
 H46C), C46(H46D,H46E,H46F)
;
_shelx_res_checksum              35642
_shelx_hkl_checksum              22624
_olex2_submission_special_instructions 'No special instructions were received'