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_7128385
_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         'C30 H50 N4 O Sr'
_chemical_formula_sum            'C30 H50 N4 O Sr'
_chemical_formula_weight         570.36
_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             2021-05-18
_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                88.58(3)
_cell_angle_beta                 87.44(3)
_cell_angle_gamma                70.78(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8102(18)
_cell_length_b                   9.0828(18)
_cell_length_c                   19.687(4)
_cell_measurement_reflns_used    46091
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.48
_cell_measurement_theta_min      2.25
_cell_volume                     1486.0(6)
_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      100.0
_diffrn_detector                 'Hybrid Pixel Counting Detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
 7622 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  0.0265
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16035
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.283
_diffrn_reflns_theta_min         2.246
_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    2.722
_exptl_absorpt_correction_T_max  0.5578
_exptl_absorpt_correction_T_min  0.1905
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       rod
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         5489
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0372P)^2^+0.2071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5064
_reflns_number_total             5489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02040d2.cif
_cod_data_source_block           jo00810neu
_cod_depositor_comments
'Adding full bibliography for 7128384--7128387.cif.'
_cod_database_code               7128385
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.496
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Rigid bond restraints
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Sof(C1B)=Sof(H1C)=Sof(H1D)=Sof(C2B)=Sof(H2C)=Sof(H2D)=Sof(C3B)=Sof(H3C)=
 Sof(H3D)=Sof(C4B)=Sof(H4C)=Sof(H4D)=Sof(C5B)=Sof(H5C)=Sof(H5D)=Sof(C6B)=
 Sof(H6C)=Sof(H6D)=Sof(C7B)=Sof(H7C)=Sof(H7D)=Sof(C8B)=Sof(H8C)=Sof(H8D)=1-
 FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(H1B)=Sof(C2A)=Sof(H2A)=Sof(H2B)=Sof(C3A)=Sof(H3A)=
 Sof(H3B)=Sof(C4A)=Sof(H4A)=Sof(H4B)=Sof(C5A)=Sof(H5A)=Sof(H5B)=Sof(C6A)=
 Sof(H6A)=Sof(H6B)=Sof(C7A)=Sof(H7A)=Sof(H7B)=Sof(C8A)=Sof(H8A)=Sof(H8B)=FVAR(1)
 Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29C)=Sof(H29D)=Sof(H30C)=Sof(H30D)=1-FVAR(2)
 Sof(H28A)=Sof(H28B)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H30A)=Sof(H30B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1A(H1A,H1B), C2A(H2A,H2B), C3A(H3A,H3B), C4A(H4A,H4B), C5A(H5A,H5B), C6A(H6A,
 H6B), C7A(H7A,H7B), C8A(H8A,H8B), C1B(H1C,H1D), C2B(H2C,H2D), C3B(H3C,H3D),
 C4B(H4C,H4D), C5B(H5C,H5D), C6B(H6C,H6D), C7B(H7C,H7D), C8B(H8C,H8D), C28(H28A,
 H28B), C28(H28C,H28D), C29A(H29A,H29B), C29B(H29C,H29D), C30(H30A,H30B),
 C30(H30C,H30D)
;
_shelx_res_checksum              17203
_shelx_hkl_checksum              73704
_olex2_submission_special_instructions 'No special instructions were received'