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_7133265
_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         '2(C62 H96 Ca2 N4 Zn2), 2(C6 H6)'
_chemical_formula_sum            'C136 H204 Ca4 N8 Zn4'
_chemical_formula_weight         2372.86
_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             2024-02-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-03 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                69.051(4)
_cell_angle_beta                 69.699(4)
_cell_angle_gamma                71.172(4)
_cell_formula_units_Z            1
_cell_length_a                   15.2503(6)
_cell_length_b                   16.0371(6)
_cell_length_c                   16.0776(6)
_cell_measurement_reflns_used    11438
_cell_measurement_temperature    149.9(7)
_cell_measurement_theta_max      29.9470
_cell_measurement_theta_min      3.2110
_cell_volume                     3354.3(3)
_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 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.856
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32763
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.205
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88317
_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    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.538
_exptl_crystal_size_mid          0.388
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         17073
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0657P)^2^+0.8019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13243
_reflns_number_total             17073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02930e2.cif
_cod_data_source_block           e24msh05
_cod_depositor_comments
'Adding full bibliography for 7133265--7133266.cif.'
_cod_database_code               7133265
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C31-H31B = C31-H31A = C31-H31C = C30-H30C = C30-H30B = C30-H30A = C61-H61C =
 C61-H61B = C61-H61A = C62-H62A = C62-H62C = C62-H62B
 0.98 with sigma of 0.005
 Zn2-Ca2 \\sim Zn2A-Ca2 \\sim Zn1A-Ca1 \\sim Zn1-Ca1
 with sigma of 0.005
3. Others
 Fixed Sof: Zn1(0.95) Zn1A(0.05) Zn2(0.95) Zn2A(0.05)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C43(H43), C46(H46), C55(H55), C58(H58)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C33(H33),
 C39(H39), C40(H40), C41(H41), C51(H51), C52(H52), C53(H53), C63(H63), C64(H64),
  C65(H65), C66(H66), C67(H67), C68(H68)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              23005
_shelx_hkl_checksum              22247
_olex2_submission_special_instructions 'No special instructions were received'