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_7134806
_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 O3, 2(C5 H12)'
_chemical_formula_sum            'C94 H158 Ca2 N4 O3'
_chemical_formula_weight         1472.39
_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                71.5478(17)
_cell_angle_beta                 72.2458(17)
_cell_angle_gamma                62.332(2)
_cell_formula_units_Z            1
_cell_length_a                   12.7723(3)
_cell_length_b                   12.8615(3)
_cell_length_c                   16.5534(3)
_cell_measurement_reflns_used    18084
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      74.3360
_cell_measurement_theta_min      3.9270
_cell_volume                     2243.75(10)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_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   -110.00 -24.00   1.00    3.00    --  -41.44 -38.00   0.00   86
  2  \w    -68.00  -9.00   1.00    3.00    --  -41.44 125.00 150.00   59
  3  \w    -65.00  17.00   1.00    3.00    --  -41.44  57.00 150.00   82
  4  \w   -115.00 -19.00   1.00    3.00    --  -41.44 -38.00 -90.00   96
  5  \w     53.00  91.00   1.00    3.00    --   41.44-125.00   0.00   38
  6  \w     53.00 106.00   1.00   12.00    --  107.95-111.00-180.00   53
  7  \w    127.00 178.00   1.00   12.00    --  107.95  77.00   0.00   51
  8  \w     72.00 128.00   1.00   12.00    --  107.95 178.00   0.00   56
  9  \w     36.00 109.00   1.00   12.00    --  107.95-111.00 120.00   73
 10  \w     30.00 153.00   1.00   12.00    --  107.95 -15.00 -90.00  123
 11  \w     42.00 109.00   1.00   12.00    --  107.95-111.00 -30.00   67
 12  \w     37.00 106.00   1.00   12.00    --  107.95 -94.00-150.00   69
 13  \w    100.00 176.00   1.00   12.00    --  107.95  45.00  90.00   76
 14  \w     42.00 132.00   1.00   12.00    --  107.95 -61.00 -60.00   90
 15  \w     32.00 123.00   1.00   12.00    --  107.95 -30.00  60.00   91
 16  \w    -87.00  -6.00   1.00    3.00    --  -41.69 125.00 -90.00   81
 17  \w   -114.00 -14.00   1.00    3.00    --  -41.69 -57.00 120.00  100
 18  \w   -114.00 -14.00   1.00    3.00    --  -41.69 -57.00-150.00  100
 19  \w     14.00 115.00   1.00    3.00    --   41.69  57.00  90.00  101
 20  \w     79.00 178.00   1.00   12.00    --  107.95  61.00 -90.00   99
 21  \w     55.00 178.00   1.00   12.00    --  107.95  15.00-120.00  123
 22  \w     82.00 178.00   1.00   12.00    --  107.95  45.00  60.00   96
 23  \w     79.00 178.00   1.00   12.00    --  107.95  61.00   0.00   99
 24  \w     55.00 178.00   1.00   12.00    --  107.95  15.00   0.00  123
 25  \w     79.00 178.00   1.00   12.00    --  107.95  61.00 150.00   99
 26  \w     79.00 178.00   1.00   12.00    --  107.95  61.00-120.00   99
 27  \w     79.00 178.00   1.00   12.00    --  107.95  61.00 120.00   99
 28  \w    -87.00  -6.00   1.00    3.00    --  -41.69 125.00 -30.00   81
 29  \w     14.00  70.00   1.00    3.00    --   41.69  57.00   0.00   56
;
_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      -0.1142621000
_diffrn_orient_matrix_UB_12      -0.0246681000
_diffrn_orient_matrix_UB_13      0.0391073000
_diffrn_orient_matrix_UB_21      -0.0281121000
_diffrn_orient_matrix_UB_22      0.0621615000
_diffrn_orient_matrix_UB_23      0.0744310000
_diffrn_orient_matrix_UB_31      -0.0733568000
_diffrn_orient_matrix_UB_32      0.1210006000
_diffrn_orient_matrix_UB_33      -0.0539343000
_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  0.0267
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.394
_diffrn_reflns_theta_min         2.865
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.655
_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    1.090
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8939
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0590P)^2^+1.1679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7915
_reflns_number_total             8939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03340c2.cif
_cod_data_source_block           hasj220112b
_cod_depositor_comments
'Adding full bibliography for 7134806--7134807.cif.'
_cod_original_cell_volume        2243.75(9)
_cod_database_code               7134806
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C94H158Ca2N4O3
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.700
_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. Restrained distances
 C52-C51 \\sim C51-C50 \\sim C49-C50 \\sim C49-C48 \\sim C47-C46 \\sim C45-C46
\\sim C45-C44 \\sim C43-C44
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C48, C49, C50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C43(0.5) H43a(0.5) H43b(0.5) H43c(0.5) C44(0.5) H44a(0.5)
 H44b(0.5) C45(0.5) H45a(0.5) H45b(0.5) C46(0.5) H46a(0.5) H46b(0.5) C47(0.5)
 H47a(0.5) H47b(0.5) H47c(0.5) C48(0.5) H48a(0.5) H48b(0.5) H48c(0.5) C49(0.5)
 H49a(0.5) H49b(0.5) C50(0.5) H50a(0.5) H50b(0.5) C51(0.5) H51a(0.5) H51b(0.5)
 C52(0.5) H52a(0.5) H52b(0.5) H52c(0.5)
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), C46(H46a,H46b), C49(H49a,H49b), C50(H50a,H50b), C51(H51a,H51b)
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), C47(H47a,
 H47b,H47c), C48(H48a,H48b,H48c), C52(H52a,H52b,H52c)
;
_shelx_res_checksum              85604
_shelx_hkl_checksum              95576
_olex2_date_sample_data_collection 2022-01-12
_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 4.743
_oxdiff_exptl_absorpt_empirical_full_min 0.641