Low-coordinate calcium peroxide and oxide complexes.
Thum, Stefan; Schmidt, Marcel A.; Langer, Jens; Harder, Sjoerd; Chemical communications (Cambridge, England) 61 (2025) 12127–12130; doi:10.1039/d5cc03340c

data_7134807
_publ_section_title
;
 Low-coordinate calcium peroxide and oxide complexes.
;
_journal_issue                   65
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12127
_journal_page_last               12130
_journal_paper_doi               10.1039/d5cc03340c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C84 H134 Ca2 N4 O4, C6 H14, 1[C6H14]'
_chemical_formula_sum            'C96 H162 Ca2 N4 O4'
_chemical_formula_weight         1516.45
_chemical_properties_physical    Moisture-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-27 deposited with the CCDC.	2025-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                71.9328(16)
_cell_angle_beta                 71.5933(19)
_cell_angle_gamma                62.498(2)
_cell_formula_units_Z            1
_cell_length_a                   12.8220(3)
_cell_length_b                   12.8590(2)
_cell_length_c                   16.6221(3)
_cell_measurement_reflns_used    21002
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      72.6950
_cell_measurement_theta_min      3.9150
_cell_volume                     2262.16(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.978
_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    -70.00  32.00   1.00    1.00    --  -41.44  57.00 -60.00  102
  2  \w    -74.00  35.00   1.00    1.00    --  -41.44  77.00  60.00  109
  3  \w   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00 150.00  101
  4  \w    103.00 178.00   1.00    3.00    --  104.37  77.00-120.00   75
  5  \w    103.00 178.00   1.00    3.00    --  104.37  77.00-150.00   75
  6  \w    103.00 178.00   1.00    3.00    --  104.37  77.00  30.00   75
  7  \w     32.00 133.00   1.00    3.00    --  104.37 -61.00-120.00  101
  8  \w     31.00 112.00   1.00    3.00    --  104.37-125.00  60.00   81
  9  \w     31.00 130.00   1.00    3.00    --  104.37 -45.00  90.00   99
 10  \w     22.00 106.00   1.00    3.00    --  104.37 -94.00  60.00   84
 11  \w     22.00 106.00   1.00    3.00    --  104.37 -94.00 150.00   84
 12  \w     31.00 112.00   1.00    3.00    --  104.37-125.00 -90.00   81
 13  \w     52.00 178.00   1.00    3.00    --  104.37  15.00   0.00  126
 14  \w   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00-150.00  101
 15  \w   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00  30.00  101
 16  \w   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00 -60.00  101
 17  \w     75.00 177.00   1.00    3.00    --  104.37  61.00-120.00  102
 18  \w     75.00 177.00   1.00    3.00    --  104.37  61.00  60.00  102
 19  \w     75.00 177.00   1.00    3.00    --  104.37  61.00-180.00  102
 20  \w     75.00 177.00   1.00    3.00    --  104.37  61.00  90.00  102
 21  \w     75.00 177.00   1.00    3.00    --  104.37  61.00   0.00  102
 22  \w     75.00 177.00   1.00    3.00    --  104.37  61.00-150.00  102
 23  \w     75.00 177.00   1.00    3.00    --  104.37  61.00  30.00  102
 24  \w     52.00 178.00   1.00    3.00    --  104.37  15.00-180.00  126
;
_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      -0.0147153000
_diffrn_orient_matrix_UB_12      -0.0430415000
_diffrn_orient_matrix_UB_13      0.0987447000
_diffrn_orient_matrix_UB_21      0.0532115000
_diffrn_orient_matrix_UB_22      -0.1303637000
_diffrn_orient_matrix_UB_23      -0.0115645000
_diffrn_orient_matrix_UB_31      0.1268947000
_diffrn_orient_matrix_UB_32      -0.0109045000
_diffrn_orient_matrix_UB_33      -0.0059237000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34013
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.684
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.113
_exptl_crystal_description       block
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.161
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8804
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0410P)^2^+0.6345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8412
_reflns_number_total             8804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03340c2.cif
_cod_data_source_block           hasj211028b
_cod_depositor_comments
'Adding full bibliography for 7134806--7134807.cif.'
_cod_original_cell_volume        2262.16(10)
_cod_database_code               7134807
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C96Ca2H162N4O4
_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
 C44-C45 \\sim C45A-C44A \\sim C43-C44 \\sim C43-C44A \\sim C45A-C45A_$2 \\sim
C45-C45_$2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C44A \\sim C45A: within 4A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 4A
4. Others
 Sof(H43d)=Sof(H43e)=Sof(H43f)=Sof(C44A)=Sof(H44c)=Sof(H44d)=Sof(C45A)=
 Sof(H45c)=Sof(H45d)=1-FVAR(1)
 Sof(H43a)=Sof(H43b)=Sof(H43c)=Sof(C44)=Sof(H44a)=Sof(H44b)=Sof(C45)=Sof(H45a)=
 Sof(H45b)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C17(H17), C28(H28), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C15(H15a,H15b), C18(H18a,H18b), C20(H20a,H20b), C29(H29a,
 H29b), C31(H31a,H31b), C34(H34a,H34b), C36(H36a,H36b), C38(H38a,H38b),
 C39(H39a,H39b), C40(H40a,H40b), C41(H41a,H41b), C42(H42a,H42b), C44(H44a,H44b),
  C45(H45a,H45b), C44A(H44c,H44d), C45A(H45c,H45d)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C14(H14a,H14b,H14c), C16(H16a,H16b,H16c),
 C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C30(H30a,H30b,H30c), C32(H32a,H32b,
 H32c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C43(H43a,H43b,H43c), C43(H43d,
 H43e,H43f)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96136
_shelx_hkl_checksum              4078
_shelx_fab_checksum              22600
_olex2_date_sample_data_collection 2021-10-28
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.259
_oxdiff_exptl_absorpt_empirical_full_min 0.834