Pathway to a molecular calcium methyl.
Pearce, Kyle G.; Neale, Samuel E.; McMullin, Claire L.; Mahon, Mary F.; Hill, Michael S.; Chemical communications (Cambridge, England) 60 (2024) 7882–7885; doi:10.1039/d4cc02930e

data_7133266
_publ_section_title
;
 Pathway to a molecular calcium methyl.
;
_journal_issue                   61
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7882
_journal_page_last               7885
_journal_paper_doi               10.1039/d4cc02930e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C60 H88 Ca2 N4, 2(C6 H14)'
_chemical_formula_sum            'C72 H116 Ca2 N4'
_chemical_formula_weight         1117.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-03 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.430(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5951(4)
_cell_length_b                   19.1092(4)
_cell_length_c                   14.1535(4)
_cell_measurement_reflns_used    7345
_cell_measurement_temperature    149.9(7)
_cell_measurement_theta_max      29.6270
_cell_measurement_theta_min      3.2880
_cell_volume                     3488.37(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.9(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34856
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.387
_diffrn_reflns_theta_min         3.034
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.319
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         9311
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0869P)^2^+1.5942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6486
_reflns_number_total             9311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02930e2.cif
_cod_data_source_block           e24msh09
_cod_depositor_comments
'Adding full bibliography for 7133265--7133266.cif.'
_cod_database_code               7133266
_shelx_shelxl_version_number     2019/3
_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
 C30-H30C = C30-H30B = C30-H30A
 0.98 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
H30A \\sim H30B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
4. Rigid body (RIGU) restrains
 C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C15(H15), C24(H24), C27(H27), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C33(H33A,H33B), C35(H35A,H35B), C32(H32A,H32B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C8(H8), C20(H20), C22(H22), C9(H9), C21(H21)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C16(H16A,H16B,H16C), C13(H13A,H13B,H13C),
 C25(H25A,H25B,H25C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C26(H26A,H26B,
 H26C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C36(H36A,H36B,H36C), C31(H31A,
 H31B,H31C)
;
_shelx_res_checksum              87757
_shelx_hkl_checksum              87336
_olex2_submission_special_instructions 'No special instructions were received'