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_7128386
_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(C28 H66 Ca1.23 N8 O Sr0.77), 4(C32 H36 B), 5(C4 H8 O)'
_chemical_formula_sum            'C204 H316 B4 Ca2.52 N16 O7 Sr1.49'
_chemical_formula_weight         3378.87
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-05-17
_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                90
_cell_angle_beta                 101.7303(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.3924(3)
_cell_length_b                   12.75071(15)
_cell_length_c                   35.5684(4)
_cell_measurement_reflns_used    58965
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.58
_cell_measurement_theta_min      4.31
_cell_volume                     9943.4(2)
_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                 'Hybrid Pixel Counting Detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
 4219 frames, detector distance = 65 mm
;
_diffrn_measurement_device       '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  0.0581
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            65203
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.822
_diffrn_reflns_theta_min         4.307
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_target            Cu
_diffrn_source_type              'Xenocs Cu microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.539
_exptl_absorpt_correction_T_max  0.0544
_exptl_absorpt_correction_T_min  0.0124
_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            colorless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       rod
_exptl_crystal_F_000             3669
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         18680
_refine_ls_number_restraints     1060
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11925
_reflns_number_total             18680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02040d2.cif
_cod_data_source_block           jo00717neu
_cod_depositor_comments
'Adding full bibliography for 7128384--7128387.cif.'
_cod_database_code               7128386
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.557
_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. Shared sites
{Sr1, Ca2}
3. Uiso/Uaniso restraints and constraints
Uanis(Sr1) = Uanis(Ca2)
4. 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
5. Others
 Sof(Ca2)=1-FVAR(1)
 Sof(Sr1)=FVAR(1)
 Sof(N5B)=Sof(N6B)=Sof(N7B)=Sof(N8B)=Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C14B)=
 Sof(H14C)=Sof(H14D)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(H16C)=
 Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(H18C)=Sof(H18D)=
 Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=
 Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=1-FVAR(2)
 Sof(N5A)=Sof(N6A)=Sof(N7A)=Sof(N8A)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C14A)=
 Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(H16A)=
 Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=
 Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(C21A)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(2)
 Sof(O1B)=Sof(C25B)=Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26C)=Sof(H26D)=
 Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28C)=Sof(H28D)=1-FVAR(3)
 Sof(O1A)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=
 Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=FVAR(3)
 Fixed Sof: O4(0.5) C101(0.5) H103(0.5) H104(0.5) C102(0.5) H105(0.5)
 H106(0.5) C103(0.5) H107(0.5) H108(0.5) C104(0.5) H109(0.5) H110(0.5)
 Fixed Uiso: H1(0.05) H2(0.05)
6.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), C13A(H13A,H13B), C14A(H14A,H14B), C15A(H15A,H15B),
 C16A(H16A,H16B), C17A(H17A,H17B), C18A(H18A,H18B), C19A(H19A,H19B), C20A(H20A,
 H20B), C25A(H25A,H25B), C26A(H26A,H26B), C27A(H27A,H27B), C28A(H28A,H28B),
 C13B(H13C,H13D), C14B(H14C,H14D), C15B(H15C,H15D), C16B(H16C,H16D), C17B(H17C,
 H17D), C18B(H18C,H18D), C19B(H19C,H19D), C20B(H20C,H20D), C25B(H25C,H25D),
 C26B(H26C,H26D), C27B(H27C,H27D), C28B(H28C,H28D), C93(H93A,H93B), C94(H94A,
 H94B), C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B),
 C99(H99A,H99B), C100(H101,H102), C101(H103,H104), C102(H105,H106), C103(H107,
 H108), C104(H109,H110)
6.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C21A(H21A,H21B,H21C), C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C),
 C24A(H24A,H24B,H24C), C21B(H21D,H21E,H21F), C22B(H22D,H22E,H22F), C23B(H23D,
 H23E,H23F), C24B(H24D,H24E,H24F), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C91(H91A,H91B,H91C),
 C92(H92A,H92B,H92C)
6.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C32(H32), C34(H34), C38(H38), C40(H40), C42(H42), C46(H46),
 C48(H48), C50(H50), C54(H54), C56(H56), C58(H58), C62(H62), C64(H64), C66(H66),
  C70(H70), C72(H72), C74(H74), C78(H78), C80(H80), C82(H82), C86(H86),
 C88(H88), C90(H90)
6.d Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C)
;
_shelx_res_checksum              86587
_shelx_hkl_checksum              66116
_olex2_submission_special_instructions 'No special instructions were received'