Large decanuclear calcium and strontium hydride clusters.
Martin, Johannes; Eyselein, Jonathan; Langer, Jens; Elsen, Holger; Harder, Sjoerd; Chemical communications (Cambridge, England) 56 (2020) 9178–9181; doi:10.1039/d0cc04330c

data_7126808
_publ_section_title
;
 Large decanuclear calcium and strontium hydride clusters.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9178
_journal_page_last               9181
_journal_paper_doi               10.1039/d0cc04330c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C102 H214 Ca10 N10 Si4'
_chemical_formula_sum            'C102 H214 Ca10 N10 Si4'
_chemical_formula_weight         2093.98
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-02
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2019-12-09 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   46.5535(3)
_cell_length_b                   46.5535(3)
_cell_length_c                   18.2299(2)
_cell_measurement_reflns_used    30087
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.6050
_cell_measurement_theta_min      4.6120
_cell_volume                     34215.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -121.00   0.00   1.00    4.00    --  -41.44 -19.00  60.00  121
  2  \w     74.00 177.00   1.00   16.00    --  104.37  66.00-177.00  103
  3  \w     32.00 133.00   1.00   16.00    --  104.37 -61.00 -90.00  101
  4  \w    104.00 178.00   1.00   16.00    --  104.37  91.00  40.00   74
  5  \w   -116.00 -17.00   1.00    4.00    --  -41.44 -38.00 -60.00   99
  6  \w     27.00  97.00   1.00    4.00    --   41.44-125.00-180.00   70
  7  \w    103.00 178.00   1.00   16.00    --  104.37  77.00 -30.00   75
  8  \w     31.00 112.00   1.00   16.00    --  104.37-125.00 150.00   81
  9  \w     79.00 177.00   1.00   16.00    --  104.37  45.00 120.00   98
 10  \w     79.00 177.00   1.00   16.00    --  104.37  45.00 -90.00   98
 11  \w   -114.00 -25.00   1.00    4.00    --  -41.44 -57.00-150.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0120304000
_diffrn_orient_matrix_UB_12      0.0216358000
_diffrn_orient_matrix_UB_13      -0.0380901000
_diffrn_orient_matrix_UB_21      0.0263943000
_diffrn_orient_matrix_UB_22      0.0090862000
_diffrn_orient_matrix_UB_23      -0.0602355000
_diffrn_orient_matrix_UB_31      -0.0248326000
_diffrn_orient_matrix_UB_32      -0.0301307000
_diffrn_orient_matrix_UB_33      -0.0455118000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            70540
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.792
_diffrn_reflns_theta_min         3.781
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.575
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.915
_exptl_crystal_description       block
_exptl_crystal_F_000             10368
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.185
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         14967
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0605P)^2^+69.4555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13608
_reflns_number_total             14967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04330c2.cif
_cod_data_source_block           hasj191001a
_cod_depositor_comments
'Adding full bibliography for 7126808--7126809.cif.'
_cod_original_cell_volume        34215.2(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7126808
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C120H240Ca10N10Si4
_shelx_estimated_absorpt_t_max   0.558
_shelx_estimated_absorpt_t_min   0.374
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C15-C13 \\sim C15-C13A \\sim C14A-C13A \\sim C14-C13 \\sim C9A-C7A \\sim C9-C7
\\sim C8-C7 \\sim C8A-C7A
 with sigma of 0.02
 Si1-C13A \\sim Si1-C13
 with sigma of 0.02
 C7A-C2 \\sim C7-C2
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C9 \\sim C7A \\sim C8A \\sim C9A: within 3A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 3A
4. Rigid body (RIGU) restrains
 C15, C7, C8, C9, C7A, C8A, C9A, C13A, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=FVAR(1)
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C16(H16), C19(H19), C28(H28), C31(H31), C34(H34), C37(H37),
 C40(H40), C7(H7), C13(H13), C7A(H7A), C13A(H13A)
6.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C46(H46A,H46B), C48(H48A,H48B), C49(H49A,H49B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C24(H24), C25(H25), C26(H26)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C15(H15D,H15E,
 H15F), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C),
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C14A(H14D,H14E,H14F)
;
_olex2_date_sample_data_collection 2019-10-01
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.803