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_7047261
_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         'C35 H47 Ca N2, Al C16 F36 O4'
_chemical_formula_sum            'C51 H47 Al Ca F36 N2 O4'
_chemical_formula_weight         1502.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-07 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.767(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9248(10)
_cell_length_b                   24.8726(10)
_cell_length_c                   12.2476(6)
_cell_measurement_reflns_used    4632
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      68.1170
_cell_measurement_theta_min      4.2250
_cell_volume                     6191.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0404
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20064
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.507
_diffrn_reflns_theta_min         2.808
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         5829
_refine_ls_number_restraints     455
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0764
_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^)+(0.1170P)^2^+15.4038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4170
_reflns_number_total             5829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03124j2.cif
_cod_data_source_block           s17msh154
_cod_depositor_comments
'Adding full bibliography for 7047260--7047266.cif.'
_cod_database_code               7047261
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 O1_2-C1_2
 1.35 with sigma of 0.02
 C1_2-C2_2 \\sim C1_2-C3_2 \\sim C1_2-C4_2
 with sigma of 0.02
 F1_2-C2_2 \\sim F2_2-C2_2 \\sim F3_2-C2_2 \\sim F4_2-C3_2 \\sim F5_2-C3_2
\\sim F6_2-C3_2 \\sim F7_2-
 C4_2 \\sim F8_2-C4_2 \\sim F9_2-C4_2
 with sigma of 0.02
 C2_2-C3_2 \\sim C3_2-C4_2 \\sim C2_2-C4_2
 with sigma of 0.04
 O1_2-C2_2 \\sim O1_2-C3_2 \\sim O1_2-C4_2
 with sigma of 0.04
 F1_2-F2_2 \\sim F2_2-F3_2 \\sim F3_2-F1_2 \\sim F4_2-F5_2 \\sim F5_2-F6_2
\\sim F6_2-F4_2 \\sim F7_2-
 F8_2 \\sim F8_2-F9_2 \\sim F9_2-F7_2
 with sigma of 0.04
 F1_2-C1_2 \\sim F2_2-C1_2 \\sim F3_2-C1_2 \\sim F4_2-C1_2 \\sim F5_2-C1_2
\\sim F6_2-C1_2 \\sim F7_2-
 C1_2 \\sim F8_2-C1_2 \\sim F9_2-C1_2
 with sigma of 0.1
 F3A-C2A \\sim F3_3-C2_3 \\sim F1A-C2A \\sim F1_3-C2_3 \\sim F2A-C2A \\sim
F2_3-C2_3
 with sigma of 0.01
 C2A-C1_3 \\sim C2_3-C1_3
 with sigma of 0.005
 F1-C3_3 \\sim F5_3-C3_3 \\sim F3-C3_3 \\sim F4_3-C3_3
 with sigma of 0.005
 F2_4-C2_4 \\sim F1_4-C2_4 \\sim F3_4-C2_4 \\sim F4_4-C3_4 \\sim F6_4-C3_4
\\sim F5_4-C3_4 \\sim F8_4-
 C4_4 \\sim F9_4-C4_4 \\sim F7_4-C4_4
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O1_2 \\sim C1_2 \\sim C2_2 \\sim F1_2 \\sim F2_2 \\sim F3_2 \\sim C3_2 \\sim
F4_2 \\sim F5_2 \\sim F6_2 \\sim C4_2 \\sim F7_2 \\sim F8_2 \\sim F9_2: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F4_3 \\sim F1 \\sim F5_3 \\sim F3: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.01
Uanis(C1_1) = Uanis(C1_2)
4. Rigid body (RIGU) restrains
 F1_2, F2_2, F3_2, F4_2, F5_2, F6_2, F7_2, F8_2, F9_2, O1_2, C1_2, C2_2, C3_2,
 C4_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1A, F2A, F3A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1_3, F2_3, F3_3, C2_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4_4, F5_4, F6_4, C3_4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7_4, F8_4, F9_4, C4_4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F1A(0.45) F2A(0.45) F3A(0.45) C2A(0.45) F1(0.25) F3(0.5) F1(0.55)
 F2(0.55) F3(0.55) F4(0.55) F5(0.55) F6(0.55) F7(0.55) F8(0.55) F9(0.55)
 O1(0.55) C1(0.55) C2(0.55) C3(0.55) C4(0.55) F1(0.45) F2(0.45) F3(0.45)
 F4(0.45) F5(0.45) F6(0.45) F7(0.45) F8(0.45) F9(0.45) O1(0.45) C1(0.45)
 C2(0.45) C3(0.45) C4(0.45) F1(0.55) F2(0.55) F3(0.55) F4(0.25) F5(0.5)
 C2(0.55) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) F7(0.5) F8(0.5) F9(0.5)
 C2(0.5) C3(0.5) C4(0.5)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C16(H16), C17(H17), C18(H18)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'