A Tetranuclear Calcium Hydride Cluster with a Highly Symmetric [Ca4H6]2+ Core
Okuda, Jun; Schuhknecht, Danny; Spaniol, Thomas Paul; Laurent, Maron; Douair, Iskander; Chemical Communications  (2019) –; doi:10.1039/C9CC08540H

data_7124522
_publ_section_title
;
 A Tetranuclear Calcium Hydride Cluster with a Highly Symmetric [Ca4H6]2+
 Core
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC08540H
_journal_year                    2019
_chemical_formula_moiety         'C32 H36 B,  C18 H45 Ca2 N6, 2(C4 H8 O)'
_chemical_formula_sum            'C58 H97 B Ca2 N6 O2'
_chemical_formula_weight         1001.38
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-28 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.88272(18)
_cell_length_b                   18.88272(18)
_cell_length_c                   16.61907(16)
_cell_measurement_reflns_used    108320
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.57
_cell_measurement_theta_min      3.31
_cell_volume                     5925.65(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
 6573 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  0.0582
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61098
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.993
_diffrn_reflns_theta_min         3.310
_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    1.996
_exptl_absorpt_correction_T_max  0.5278
_exptl_absorpt_correction_T_min  0.3591
_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    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_recrystallization_method 'from the reaction mixture in thf'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 2412 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5788
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+3.9246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                5590
_reflns_number_total             5788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08540h2.cif
_cod_data_source_block           2
_cod_original_cell_volume        5925.65(13)
_cod_database_code               7124522
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.657
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H4A,H4B} of C4, {H5A,H5B} of C5, {H6A,H6B} of C6, {H26A,
  H26B} of C26A, {H28A,H28B} of C28A, {H27A,H27B} of C27A, {H29A,H29B} of C29A,
  {H27C,H27D} of C27B, {H26C,H26D} of C26B, {H28C,H28D} of C28B, {H29C,H29D} of
  C29B, {H2A,H2B} of C2, {H1A,H1B} of C1, {H3A,H3B} of C3
 At 1.5 times of:
  All C(H,H,H) groups, {H25A,H25B} of C25
2. Restrained distances
 O1A-C26A
 1.4 with sigma of 0.02
 O1A-C29A
 1.4 with sigma of 0.02
 C26A-C27A
 1.5 with sigma of 0.02
 C27A-C28A
 1.5 with sigma of 0.02
 C28A-C29A
 1.5 with sigma of 0.02
 O1A-C27A
 -2.2 with sigma of 0.02
 O1A-C28A
 -2.2 with sigma of 0.02
 C26A-C28A
 -2.2 with sigma of 0.02
 C26A-C29A
 -2.2 with sigma of 0.02
 C27A-C29A
 -2.2 with sigma of 0.02
 C28A-O1A
 -2.2 with sigma of 0.02
 O1B-C26B
 1.4 with sigma of 0.02
 O1B-C29B
 1.4 with sigma of 0.02
 C26B-C27B
 1.5 with sigma of 0.02
 C27B-C28B
 1.5 with sigma of 0.02
 C28B-C29B
 1.5 with sigma of 0.02
 O1B-C27B
 -2.2 with sigma of 0.02
 O1B-C28B
 -2.2 with sigma of 0.02
 C26B-C28B
 -2.2 with sigma of 0.02
 C26B-C29B
 -2.2 with sigma of 0.02
 C27B-C29B
 -2.2 with sigma of 0.02
 C28B-O1B
 -2.2 with sigma of 0.02
3. Others
 Sof(O1B)=Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)=
 Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29C)=Sof(H29D)=1-FVAR(1)
 Sof(O1A)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=
 Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(C29A)=Sof(H29A)=Sof(H29B)=FVAR(1)
4.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),
 C26A(H26A,H26B), C27A(H27A,H27B), C28A(H28A,H28B), C29A(H29A,H29B), C26B(H26C,
 H26D), C27B(H27C,H27D), C28B(H28C,H28D), C29B(H29C,H29D)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C15(H15), C19(H19), C21(H21), C23(H23)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_olex2_submission_special_instructions 'No special instructions were received'