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_7128387
_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
'2(C40 H95.97 I0.03 N12 O Sr3), 4(C32 H36 B), 5(C4 H8 O)'
_chemical_formula_sum            'C228 H375.93 B4 I0.07 N24 O7 Sr6'
_chemical_formula_weight         4143.28
_chemical_name_common            'compound 4'
_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
_audit_creation_date             2021-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-21 deposited with the CCDC.	2021-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                109.8730(12)
_cell_angle_beta                 90.2679(12)
_cell_angle_gamma                90.7112(12)
_cell_formula_units_Z            2
_cell_length_a                   17.2794(2)
_cell_length_b                   24.7939(4)
_cell_length_c                   28.3335(5)
_cell_measurement_reflns_used    87938
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.45
_cell_measurement_theta_min      2.56
_cell_volume                     11414.5(3)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.131.0 (STOE, 2017)
;
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area LANA 1.71.4.0 (STOE, 2017)
;
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_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 0.961
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details
;
 6550 frames, detector distance = 65 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  0.0311
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            100682
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.041
_diffrn_reflns_theta_min         2.557
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.285
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             4439
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.028
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2268
_refine_ls_number_reflns         42045
_refine_ls_number_restraints     2321
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0768P)^2^+36.3683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31137
_reflns_number_total             42045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02040d2.cif
_cod_data_source_block           4revised
_cod_depositor_comments
'Adding full bibliography for 7128384--7128387.cif.'
_cod_database_code               7128387
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.726
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N6-C15
 1.45 with sigma of 0.02
 N7A-C17A = N7B-C17B = N7A-C16 = N7B-C16 = N7A-C23A = N7B-C23B = N8-C18A
 1.45 with sigma of 0.02
 N8-C18B
 1.45 with sigma of 0.02
 N8-C19A = N8-C19B
 1.45 with sigma of 0.02
 N8-C24A = N8-C24B
 1.45 with sigma of 0.02
 C17A-C18A = C17B-C18B = C19A-C20 = C19B-C20
 1.5 with sigma of 0.02
 C17A-C23A = C17B-C23B = C18A-C19A = C18B-C19B
 -2.4 with sigma of 0.02
 C18A-C24A = C19A-C24A = C18B-C24B = C19B-C24B
 -2.4 with sigma of 0.02
 N8-C18A \\sim N8-C18B
 with sigma of 0.04
 N8-C19A \\sim N8-C19B
 with sigma of 0.04
 C19A-C20 \\sim C19B-C20
 with sigma of 0.04
 Sr1-H1 \\sim Sr2-H1 \\sim Sr1-H2 \\sim Sr3-H2 \\sim Sr2-H3 \\sim Sr3-H3 \\sim
Sr2-H4 \\sim Sr3-H4 \\sim Sr4-
 H5 \\sim Sr5-H5 \\sim Sr4-H6 \\sim Sr6-H6 \\sim Sr5-H7 \\sim Sr6-H7 \\sim
Sr5-H8 \\sim Sr6-H8
 with sigma of 0.02
 Sr2-I4 \\sim Sr3-I4
 with sigma of 0.02
 Sr5-I7 \\sim Sr6-I7
 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(H16C)=Sof(H16D)=Sof(N7B)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=
 Sof(H18C)=Sof(H18D)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(H20C)=Sof(H20D)=
 Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(N7A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H20A)=Sof(H20B)=
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(1)
 Sof(I7)=1-FVAR(2)
 Sof(H7)=FVAR(2)
 Uiso(H1)=Uiso(H2)=Uiso(H3)=Uiso(H4)=Uiso(I4)=Uiso(H5)=Uiso(H6)=Uiso(H7)=
 Uiso(I7)=Uiso(H8)=FVAR(3)
 Uiso(N7A)=Uiso(C17A)=Uiso(C18A)=Uiso(C19A)=Uiso(N7B)=Uiso(C17B)=Uiso(C18B)=
 Uiso(C19B)=Uiso(C23A)=Uiso(C24A)=Uiso(C23B)=Uiso(C24B)=FVAR(4)
 Sof(I4)=1-FVAR(5)
 Sof(H4)=FVAR(5)
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), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C16(H16C,H16D), C17A(H17A,H17B), C18A(H18A,H18B), C19A(H19A,
 H19B), C17B(H17C,H17D), C18B(H18C,H18D), C19B(H19C,H19D), C20(H20A,H20B),
 C20(H20C,H20D), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
  C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C105(H10J,H10K),
 C106(H10L,H10M), C107(H10N,H10O), C108(H10P,H10Q), C109(H10R,H10S), C110(H11D,
 H11E), C111(H11F,H11G), C112(H11H,H11I), C117(H11V,H11W), C118(H11X,H11Y),
 C119(H11Z,H19Z), C120(H12D,H12E), C121(H12F,H12G), C122(H12H,H12I), C123(H12J,
 H12K), C124(H12L,H12M), C129(H12Z,H19Y), C130(H13C,H13D), C131(H13E,H13F),
 C132(H13G,H13H), C133(H13I,H13J), C134(H13K,H13L), C135(H13M,H13N), C136(H13O,
 H13P), C141(H14F,H14G), C142(H14H,H14I), C143(H14J,H14K), C144(H14L,H14M)
5.b Me refined with riding coordinates:
 C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C), C23B(H23D,H23E,H23F), C24B(H24D,
 H24E,H24F)
5.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C44(H44), C46(H46), C50(H50), C52(H52), C54(H54), C58(H58),
 C60(H60), C62(H62), C66(H66), C68(H68), C70(H70), C74(H74), C76(H76), C78(H78),
  C82(H82), C84(H84), C86(H86), C90(H90), C92(H92), C94(H94), C98(H98),
 C100(H100), C102(H102), C146(H146), C148(H148), C150(H150), C154(H154),
 C156(H156), C158(H158), C162(H162), C164(H164), C166(H166), C170(H170),
 C172(H172), C174(H174), C178(H178), C180(H180), C182(H182), C186(H186),
 C188(H188), C190(H190), C194(H194), C196(H196), C198(H198), C202(H202),
 C204(H204), C206(H206)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C79(H79A,
 H79B,H79C), C80(H80A,H80B,H80C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C),
 C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C103(H10D,H10E,H10F), C104(H10G,H10H,
 H10I), C113(H11J,H11K,H11L), C114(H11M,H11N,H11O), C115(H11P,H11Q,H11R),
 C116(H11S,H11T,H11U), C125(H12N,H12O,H12P), C126(H12Q,H12R,H12S), C127(H12T,
 H12U,H12V), C128(H12W,H12X,H12Y), C137(H13Q,H13R,H13S), C138(H13T,H13U,H13V),
 C139(H13W,H13X,H13Y), C140(H14C,H14D,H14E), C151(H15C,H15D,H15E), C152(H15F,
 H15G,H15H), C159(H15I,H15J,H15K), C160(H16E,H16F,H16G), C167(H16H,H16I,H16J),
 C168(H16K,H16L,H16M), C175(H17E,H17F,H17G), C176(H17H,H17I,H17J), C183(H18E,
 H18F,H18G), C184(H18H,H18I,H18J), C191(H19E,H19F,H19G), C192(H19H,H19I,H19J),
 C199(H19K,H19L,H19M), C200(H20E,H20F,H20G), C207(H20H,H20I,H20J), C208(H20K,
 H20L,H20M)
;
_shelx_res_checksum              95784
_shelx_hkl_checksum              55148
_shelx_fab_checksum              62018
_olex2_submission_special_instructions 'No special instructions were received'