C-H and C-F coordination of arenes in neutral alkaline earth metal complexes.
McMullen, Jacob S.; Edwards, Alison J.; Hicks, Jamie; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8685–8689; doi:10.1039/d1dt01532j

data_7707660
_publ_section_title
;
 C-H and C-F coordination of arenes in neutral alkaline earth metal
 complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8685
_journal_page_last               8689
_journal_paper_doi               10.1039/d1dt01532j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C59 H74 Ca N2 O, 2(C6 H6)'
_chemical_formula_sum            'C71 H86 Ca N2 O'
_chemical_formula_weight         1023.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-12 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.11790(10)
_cell_length_b                   11.36910(10)
_cell_length_c                   26.1145(3)
_cell_measurement_reflns_used    11178
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.6550
_cell_measurement_theta_min      5.1510
_cell_volume                     3003.99(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8.1297
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19970
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.744
_diffrn_reflns_theta_min         3.888
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       plate
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 5189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.234(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         11788
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+1.8650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.867
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                11596
_reflns_number_total             11788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01532j2.cif
_cod_data_source_block           53jhjh20mono
_cod_depositor_comments
'Adding full bibliography for 7707658--7707664.cif.'
_cod_database_code               7707660
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.783
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5367(18)
 0.4633(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C14-C15 = C14-C16 = C14-C17 = C14-C15A = C14-C16A = C14-C17A
 1.53 with sigma of 0.008
 C15-C16 = C16-C17 = C17-C15 = C15A-C16A = C16A-C17A = C17A-C15A
 2.5 with sigma of 0.008
4. Uiso/Uaniso restraints and constraints
C14 \\sim C15 \\sim C16 \\sim C17 \\sim C15A \\sim C16A \\sim C17A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C45(H45), C33(H33), C42(H42)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C55(H55), C9(H9), C3(H3), C51(H51), C56(H56), C11(H11), C57(H57),
 C50(H50), C59(H59), C70(H70), C71(H71), C58(H58), C62(H62), C49(H49), C52(H52),
  C54(H54), C61(H61), C53(H53), C28(H28), C26(H26), C48(H48), C60(H60),
 C38(H38), C40(H40), C69(H69), C66(H66), C27(H27), C63(H63), C65(H65), C39(H39),
  C64(H64), C68(H68), C67(H67)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C21(H21A,H21B,H21C), C35(H35A,H35B,H35C), C43(H43A,
 H43B,H43C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C15(H15A,H15B,H15C),
 C34(H34A,H34B,H34C), C31(H31A,H31B,H31C), C47(H47A,H47B,H47C), C17(H17A,H17B,
 H17C), C23(H23A,H23B,H23C), C16A(H16D,H16E,H16F), C15A(H15D,H15E,H15F),
 C17A(H17D,H17E,H17F)
;
_shelx_res_checksum              4471
_olex2_submission_special_instructions 'No special instructions were received'