Coordination of arenes and phosphines by charge separated alkaline earth cations.
Garcia, Lucia; Anker, Mathew D.; Mahon, Mary F.; Maron, Laurent; Hill, Michael S.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12684–12693; doi:10.1039/c8dt03124j

data_7047263
_publ_section_title
;
 Coordination of arenes and phosphines by charge separated alkaline earth
 cations.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12684
_journal_page_last               12693
_journal_paper_doi               10.1039/c8dt03124j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C41 H64 Ca N2 O3, Al C16 F36 O4'
_chemical_formula_sum            'C58 H66 Al Ca F36 N2 O7.25'
_chemical_formula_weight         1658.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-18 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                73.743(2)
_cell_angle_beta                 72.551(2)
_cell_angle_gamma                88.127(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7913(3)
_cell_length_b                   15.0553(3)
_cell_length_c                   20.0086(4)
_cell_measurement_reflns_used    25525
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.0130
_cell_measurement_theta_min      3.6240
_cell_volume                     3523.38(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48376
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.161
_diffrn_reflns_theta_min         3.319
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.563
_exptl_crystal_description       needle
_exptl_crystal_F_000             1686
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1348
_refine_ls_number_reflns         14062
_refine_ls_number_restraints     1989
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0475
_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^)+(0.0718P)^2^+1.3575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12824
_reflns_number_total             14062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03124j2.cif
_cod_data_source_block           s17msh114
_cod_depositor_comments
'Adding full bibliography for 7047260--7047266.cif.'
_cod_database_code               7047263
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'colorless needles'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H30A,H30B} of C30, {H31A,H31B} of C31, {H36C,H36D} of
  C36A, {H35C,H35D} of C35A, {H32A,H32B} of C32, {H33A,H33B} of C33, {H35A,
  H35B} of C35, {H36A,H36B} of C36, {H38A,H38B} of C38, {H39A,H39B} of C39,
  {H40A,H40B} of C40, {H41A,H41B} of C41, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H17A,H17B} of C17
2. Restrained distances
 O1_5-C1_5
 O1_7-C1_7
 O1_6-C1_6
 1.35 with sigma of 0.02
 C36-C35 = C36A-C35A = C37-C36 = C37-C36A = C35-C34 = C35A-C34
 1.51 with sigma of 0.01
 C1_5-C2_5 \\sim C1_5-C3_5 \\sim C1_5-C4_5
 C1_7-C2_7 \\sim C1_7-C3_7 \\sim C1_7-C4_7
 C1_6-C2_6 \\sim C1_6-C3_6 \\sim C1_6-C4_6
 with sigma of 0.02
 F1_5-C2_5 \\sim F2_5-C2_5 \\sim F3_5-C2_5 \\sim F4_5-C3_5 \\sim F5_5-C3_5
\\sim F6_5-C3_5 \\sim F7_5-
 C4_5 \\sim F8_5-C4_5 \\sim F9_5-C4_5
 F1_7-C2_7 \\sim F2_7-C2_7 \\sim F3_7-C2_7 \\sim F4_7-C3_7 \\sim F5_7-C3_7
\\sim F6_7-C3_7 \\sim F7_7-
 C4_7 \\sim F8_7-C4_7 \\sim F9_7-C4_7
 F1_6-C2_6 \\sim F2_6-C2_6 \\sim F3_6-C2_6 \\sim F4_6-C3_6 \\sim F5_6-C3_6
\\sim F6_6-C3_6 \\sim F7_6-
 C4_6 \\sim F8_6-C4_6 \\sim F9_6-C4_6
 with sigma of 0.02
 C2_5-C3_5 \\sim C3_5-C4_5 \\sim C2_5-C4_5
 C2_7-C3_7 \\sim C3_7-C4_7 \\sim C2_7-C4_7
 C2_6-C3_6 \\sim C3_6-C4_6 \\sim C2_6-C4_6
 with sigma of 0.02
 O1_5-C2_5 \\sim O1_5-C3_5 \\sim O1_5-C4_5
 O1_7-C2_7 \\sim O1_7-C3_7 \\sim O1_7-C4_7
 O1_6-C2_6 \\sim O1_6-C3_6 \\sim O1_6-C4_6
 with sigma of 0.02
 F1_5-F2_5 \\sim F2_5-F3_5 \\sim F3_5-F1_5 \\sim F4_5-F5_5 \\sim F5_5-F6_5
\\sim F6_5-F4_5 \\sim F7_5-
 F8_5 \\sim F8_5-F9_5 \\sim F9_5-F7_5
 F1_7-F2_7 \\sim F2_7-F3_7 \\sim F3_7-F1_7 \\sim F4_7-F5_7 \\sim F5_7-F6_7
\\sim F6_7-F4_7 \\sim F7_7-
 F8_7 \\sim F8_7-F9_7 \\sim F9_7-F7_7
 F1_6-F2_6 \\sim F2_6-F3_6 \\sim F3_6-F1_6 \\sim F4_6-F5_6 \\sim F5_6-F6_6
\\sim F6_6-F4_6 \\sim F7_6-
 F8_6 \\sim F8_6-F9_6 \\sim F9_6-F7_6
 with sigma of 0.02
 F1_5-C1_5 \\sim F2_5-C1_5 \\sim F3_5-C1_5 \\sim F4_5-C1_5 \\sim F5_5-C1_5
\\sim F6_5-C1_5 \\sim F7_5-
 C1_5 \\sim F8_5-C1_5 \\sim F9_5-C1_5
 F1_7-C1_7 \\sim F2_7-C1_7 \\sim F3_7-C1_7 \\sim F4_7-C1_7 \\sim F5_7-C1_7
\\sim F6_7-C1_7 \\sim F7_7-
 C1_7 \\sim F8_7-C1_7 \\sim F9_7-C1_7
 F1_6-C1_6 \\sim F2_6-C1_6 \\sim F3_6-C1_6 \\sim F4_6-C1_6 \\sim F5_6-C1_6
\\sim F6_6-C1_6 \\sim F7_6-
 C1_6 \\sim F8_6-C1_6 \\sim F9_6-C1_6
 with sigma of 0.08
3. Uiso/Uaniso restraints and constraints
O1_5 \\sim C1_5 \\sim C2_5 \\sim F1_5 \\sim F2_5 \\sim F3_5 \\sim C3_5 \\sim
F4_5 \\sim F5_5 \\sim F6_5 \\sim C4_5 \\sim F7_5 \\sim F8_5 \\sim F9_5 \\sim
O1_7 \\sim C1_7 \\sim C2_7 \\sim F1_7 \\sim F2_7 \\sim F3_7 \\sim C3_7 \\sim
F4_7 \\sim F5_7 \\sim F6_7 \\sim C4_7 \\sim F7_7 \\sim F8_7 \\sim F9_7 \\sim
O1_6 \\sim C1_6 \\sim C2_6 \\sim F1_6 \\sim F2_6 \\sim F3_6 \\sim C3_6 \\sim
F4_6 \\sim F5_6 \\sim F6_6 \\sim C4_6 \\sim F7_6 \\sim F8_6 \\sim F9_6: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O1_2, C1_2, C2_2, F1_2, F2_2, F3_2, C3_2, F4_2, F5_2, F6_2, C4_2, F7_2, F8_2,
 F9_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_4, C1_4, C2_4, F1_4, F2_4, F3_4, C3_4, F4_4, F5_4, F6_4, C4_4, F7_4, F8_4,
 F9_4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C35, C36, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, C36A, C35A, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_5, C1_5, C2_5, F1_5, F2_5, F3_5, C3_5, F4_5, F5_5, F6_5, C4_5, F7_5, F8_5,
 F9_5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_7, C1_7, C2_7, F1_7, F2_7, F3_7, C3_7, F4_7, F5_7, F6_7, C4_7, F7_7, F8_7,
 F9_7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1_6, C1_6, C2_6, F1_6, F2_6, F3_6, C3_6, F4_6, F5_6, F6_6, C4_6, F7_6, F8_6,
 F9_6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H34A(0.35) H34B(0.35) H34C(0.65) H34D(0.65) C35(0.35) H35A(0.35)
 H35B(0.35) C36(0.35) H36A(0.35) H36B(0.35) H37A(0.35) H37B(0.35) H37C(0.65)
 H37D(0.65) O4(0.6) C36A(0.65) H36C(0.65) H36D(0.65) C35A(0.65) H35C(0.65)
 H35D(0.65) F2(0.6) F5(0.6) F1(0.6) F4(0.6) F6(0.6) F3(0.6) F7(0.6) F8(0.6)
 F9(0.6) O1(0.6) C3(0.6) C1(0.6) C2(0.6) C4(0.6) F2(0.6) F1(0.6) F6(0.6)
 F8(0.6) F7(0.6) F3(0.6) F5(0.6) F4(0.6) C4(0.6) C2(0.6) C1(0.6) C3(0.6)
 F9(0.6) F2(0.6) F1(0.6) F3(0.6) F6(0.6) F4(0.6) F5(0.6) C4(0.6) F8(0.6)
 F9(0.6) F7(0.6) C3(0.6) C1(0.6) C2(0.6) O1(0.6) O1(0.4) C1(0.4) C2(0.4)
 F1(0.4) F2(0.4) F3(0.4) C3(0.4) F4(0.4) F5(0.4) F6(0.4) C4(0.4) F7(0.4)
 F8(0.4) F9(0.4) O1(0.4) C1(0.4) C2(0.4) F1(0.4) F2(0.4) F3(0.4) C3(0.4)
 F4(0.4) F5(0.4) F6(0.4) C4(0.4) F7(0.4) F8(0.4) F9(0.4) O1(0.4) C1(0.4)
 C2(0.4) F1(0.4) F2(0.4) F3(0.4) C3(0.4) F4(0.4) F5(0.4) F6(0.4) C4(0.4)
 F7(0.4) F8(0.4) F9(0.4)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
6.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C34(H34C,H34D), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C37(H37C,H37D), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
  C36A(H36C,H36D), C35A(H35C,H35D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'