Calcium stilbene complexes: structures and dual reactivity
Causero, Andrea; Elsen, Holger; Ballmann, Gerd; Escalona, Ana; Harder, Sjoerd; Chem. Commun.  (2017) –; doi:10.1039/C7CC05792J

data_7120620
_publ_section_title
;
 Calcium stilbene complexes: structures and dual reactivity
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05792J
_journal_year                    2017
_chemical_formula_moiety         'C84 H110 Ca2 N4, 2(C6 H6)'
_chemical_formula_sum            'C96 H122 Ca2 N4'
_chemical_formula_weight         1412.13
_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
_audit_creation_date             2017-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-07-06 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.776(2)
_cell_angle_beta                 91.061(2)
_cell_angle_gamma                115.639(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3795(3)
_cell_length_b                   10.7062(4)
_cell_length_c                   20.4813(4)
_cell_measurement_reflns_used    9510
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.3280
_cell_measurement_theta_min      4.4290
_cell_volume                     1993.93(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -73.00  32.00   1.00   12.50    --  -41.69  77.00 -30.00  105
  2  \w   -114.00 -19.00   1.00   12.50    --  -41.69 -38.00  60.00   95
  3  \w    -64.00  31.00   1.00   12.50    --  -41.69  38.00-120.00   95
  4  \w     23.00  97.00   1.00   12.50    --   41.69-125.00 120.00   74
  5  \w     94.00 178.00   1.00   50.00    --  106.00 125.00  30.00   84
  6  \w     25.00 109.00   1.00   50.00    --  106.00 -94.00 120.00   84
  7  \w     35.00 130.00   1.00   50.00    --  106.00 -45.00 120.00   95
  8  \w     34.00 121.00   1.00   50.00    --  106.00-125.00  30.00   87
  9  \w     82.00 177.00   1.00   50.00    --  106.00  45.00 150.00   95
 10  \w     82.00 177.00   1.00   50.00    --  106.00  45.00-150.00   95
 11  \w     36.00 134.00   1.00   50.00    --  106.00 -61.00   0.00   98
 12  \w     25.00 109.00   1.00   50.00    --  106.00 -94.00-180.00   84
 13  \w     75.00 178.00   1.00   50.00    --  106.00  77.00  90.00  103
 14  \w   -112.00 -15.00   1.00   12.50    --  -41.69 -57.00-180.00   97
 15  \w   -112.00 -15.00   1.00   12.50    --  -41.69 -57.00   0.00   97
 16  \w   -116.00 -20.00   1.00   12.50    --  -41.69 -77.00 120.00   96
 17  \w   -112.00 -15.00   1.00   12.50    --  -41.69 -57.00 -90.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18091
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.117
_diffrn_reflns_theta_min         4.443
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       plate
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0817P)^2^+0.4017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6399
_reflns_number_total             7259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc05792j2.cif
_cod_data_source_block           hasj170224b
_cod_original_cell_volume        1993.93(11)
_cod_database_code               7120620
_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.a Ternary CH refined with riding coordinates:
 C33(H33), C11(H11), C18(H18), C6(H6), C4(H4), C30(H30), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C8(H8A,H8B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C15(H15), C37(H37), C36(H36), C40(H40), C28(H28),
 C38(H38), C39(H39), C26(H26), C27(H27), C47(H47), C48(H48), C45(H45), C46(H46),
  C43(H43), C44(H44)
2.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C)
;
_shelx_res_checksum              26011
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-02-24
_olex2_submission_original_sample_id hasj170224b
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;