Cationic strontium hydride complexes supported by an NNNN-type macrocycle.
Höllerhage, Thomas; Carpentier, Ambre; Spaniol, Thomas P.; Maron, Laurent; Englert, Ulli; Okuda, Jun; Chemical communications (Cambridge, England) 57 (2021) 6316–6319; doi:10.1039/d1cc02040d

data_7128384
_publ_section_title
;
 Cationic strontium hydride complexes supported by an NNNN-type
 macrocycle.
;
_journal_issue                   51
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6316
_journal_page_last               6319
_journal_paper_doi               10.1039/d1cc02040d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C19 H35 N4 Sr, C32 H36 B, 3(C5 H10 O1)'
_chemical_formula_sum            'C66 H101 B N4 O3 Sr'
_chemical_formula_weight         1096.93
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-16 deposited with the CCDC.	2021-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                76.2476(16)
_cell_angle_beta                 89.8441(17)
_cell_angle_gamma                86.8028(16)
_cell_formula_units_Z            2
_cell_length_a                   12.4069(3)
_cell_length_b                   13.0169(3)
_cell_length_c                   19.7043(4)
_cell_measurement_reflns_used    74685
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.24
_cell_measurement_theta_min      3.50
_cell_volume                     3086.01(12)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
 7220 frames, detector distance = 55 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36052
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.446
_diffrn_reflns_theta_min         3.501
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_correction_T_max  0.5791
_exptl_absorpt_correction_T_min  0.1072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       rod
_exptl_crystal_F_000             1184
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THP'
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.396
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.321
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         11536
_refine_ls_number_restraints     708
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.1064
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2691
_refine_ls_wR_factor_ref         0.2798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10446
_reflns_number_total             11536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02040d2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7128384--7128387.cif.'
_cod_database_code               7128384
_shelx_shelxl_version_number     2018/1
_audit_contact_author            'J. Richter'
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.553
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C64B-C0BA
 -2.4 with sigma of 0.02
 C53B-C52B
 1.5 with sigma of 0.02
 C52B-O1B
 1.5 with sigma of 0.02
 O1B-C56B
 1.5 with sigma of 0.02
 C56B-C55B
 1.5 with sigma of 0.02
 O1A-C53B
 1.45 with sigma of 0.02
 C54B-C55B
 1.45 with sigma of 0.02
 O1B-C53B
 -2.4 with sigma of 0.02
 O1B-C54B
 -2.4 with sigma of 0.02
 O1B-C55B
 -2.4 with sigma of 0.02
 C52A-C53A
 1.5 with sigma of 0.02
 C53A-C54A
 1.5 with sigma of 0.02
 C54A-C55A
 1.5 with sigma of 0.02
 C55A-C56A
 1.5 with sigma of 0.02
 O1A-C52A
 1.45 with sigma of 0.02
 C54B-C56A
 1.45 with sigma of 0.02
 C54A-C52A
 -2.4 with sigma of 0.02
 C54A-O1A
 -2.4 with sigma of 0.02
 C54A-C56A
 -2.4 with sigma of 0.02
 C53A-C55A
 -2.4 with sigma of 0.02
 C53A-C56A
 -2.4 with sigma of 0.02
 C53A-O1A
 -2.4 with sigma of 0.02
 O3A-C66A
 1.45 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O1B)=Sof(C52B)=Sof(H52C)=Sof(H52D)=Sof(C53B)=Sof(H53C)=Sof(H53D)=
 Sof(C54B)=Sof(H54C)=Sof(H54D)=Sof(C55B)=Sof(H55C)=Sof(H55D)=Sof(C56B)=
 Sof(H56C)=Sof(H56D)=1-FVAR(1)
 Sof(O1A)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(C53A)=Sof(H53A)=Sof(H53B)=
 Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(C55A)=Sof(H55A)=Sof(H55B)=Sof(C56A)=
 Sof(H56A)=Sof(H56B)=FVAR(1)
 Sof(O2B)=Sof(C57B)=Sof(H57C)=Sof(H57D)=Sof(C58B)=Sof(H58C)=Sof(H58D)=
 Sof(C59B)=Sof(H59C)=Sof(H59D)=Sof(C60B)=Sof(H60C)=Sof(H60D)=Sof(C61B)=
 Sof(H61C)=Sof(H61D)=1-FVAR(2)
 Sof(O2A)=Sof(C57A)=Sof(H57A)=Sof(H57B)=Sof(C58A)=Sof(H58A)=Sof(H58B)=
 Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(C61A)=
 Sof(H61A)=Sof(H61B)=FVAR(2)
 Sof(O3B)=Sof(C62B)=Sof(H62C)=Sof(H62D)=Sof(C63B)=Sof(H63C)=Sof(H63D)=
 Sof(C64B)=Sof(H64C)=Sof(H64D)=Sof(C65B)=Sof(H65C)=Sof(H65D)=Sof(C0BA)=
 Sof(H0BA)=Sof(H0BB)=1-FVAR(3)
 Sof(O3A)=Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(C63A)=Sof(H63A)=Sof(H63B)=
 Sof(C64A)=Sof(H64A)=Sof(H64B)=Sof(C65A)=Sof(H65A)=Sof(H65B)=Sof(C66A)=
 Sof(H66A)=Sof(H66B)=FVAR(3)
5.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), C52A(H52A,H52B), C53A(H53A,H53B), C54A(H54A,H54B),
 C55A(H55A,H55B), C56A(H56A,H56B), C52B(H52C,H52D), C53B(H53C,H53D), C54B(H54C,
 H54D), C55B(H55C,H55D), C56B(H56C,H56D), C57A(H57A,H57B), C58A(H58A,H58B),
 C59A(H59A,H59B), C60A(H60A,H60B), C61A(H61A,H61B), C57B(H57C,H57D), C58B(H58C,
 H58D), C59B(H59C,H59D), C60B(H60C,H60D), C61B(H61C,H61D), C62A(H62A,H62B),
 C63A(H63A,H63B), C64A(H64A,H64B), C65A(H65A,H65B), C66A(H66A,H66B), C62B(H62C,
 H62D), C63B(H63C,H63D), C64B(H64C,H64D), C65B(H65C,H65D), C0BA(H0BA,H0BB)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C23(H23),
 C25(H25), C29(H29), C31(H31), C33(H33), C37(H37), C39(H39), C41(H41), C45(H45),
  C47(H47), C49(H49)
5.c X=CH2 refined with riding coordinates:
 C13(H13A,H13B)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C)
;
_shelx_res_checksum              34893
_shelx_hkl_checksum              25754
_olex2_submission_special_instructions 'No special instructions were received'