Well-defined styryl and biphenyl calcium complexes from dilithio compounds and calcium iodide: synthesis, structure and reactivity toward nitrous oxide.
Wei, Baosheng; Zhang, Wen-Xiong; Xi, Zhenfeng; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12540–12545; doi:10.1039/c8dt01046c

data_7046246
_publ_section_title
;
 Well-defined styryl and biphenyl calcium complexes from dilithio
 compounds and calcium iodide: synthesis, structure and reactivity toward
 nitrous oxide.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12540
_journal_page_last               12545
_journal_paper_doi               10.1039/c8dt01046c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C44 H56 Ca2 O5'
_chemical_formula_sum            'C44 H56 Ca2 O5'
_chemical_formula_weight         745.04
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-07 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.1900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1464(3)
_cell_length_b                   14.7588(2)
_cell_length_c                   20.6595(5)
_cell_measurement_reflns_used    19617
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      28.1280
_cell_measurement_theta_min      3.5970
_cell_volume                     3973.33(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-1997 (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -26.00  58.00   0.50    2.66    --  -12.80 -19.00-180.00  168
  2  \w   -102.00 -42.00   0.50    2.66    --  -12.80 -19.00-180.00  120
  3  \w    -53.00 -27.00   0.50    2.66    --  -12.80  77.00 -90.00   52
  4  \w    -45.00 -10.00   0.50    2.66    --  -12.80  77.00  30.00   70
  5  \w    -53.00 -11.00   0.50    2.66    --  -12.80  77.00 120.00   84
  6  \w     -6.00  31.00   0.50    2.66    --  -12.80 -82.00-180.00   74
  7  \w      1.00  32.00   0.50    2.66    --  -12.80 -82.00  60.00   62
  8  \w     31.00  57.00   0.50    2.66    --   12.90 -82.00  60.00   52
  9  \w    -42.00  44.00   0.50    2.66    --   12.90 -57.00  60.00  172
 10  \w    -33.00  32.00   0.50    2.66    --   12.90 -82.00-150.00  130
 11  \w    -39.00  75.00   0.50    2.66    --   12.90  38.00  30.00  228
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0041730000
_diffrn_orient_matrix_UB_12      -0.0137337000
_diffrn_orient_matrix_UB_13      0.0404255000
_diffrn_orient_matrix_UB_21      0.0377033000
_diffrn_orient_matrix_UB_22      0.0260642000
_diffrn_orient_matrix_UB_23      0.0115257000
_diffrn_orient_matrix_UB_31      -0.0243971000
_diffrn_orient_matrix_UB_32      0.0379932000
_diffrn_orient_matrix_UB_33      0.0066454000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47278
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.395
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7796
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0541P)^2^+2.2130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6632
_reflns_number_total             7796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01046c2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7046245--7046247.cif.'
_cod_original_cell_volume        3973.32(14)
_cod_database_code               7046246
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C1 H1 O1 Ca1 I1'
_chemical_oxdiff_usercomment     ZYH171023a,Mndmen
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C32, C31, C30, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, C29, C32, C31, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C32 \\sim C31 \\sim C30 \\sim C29: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C25(H25a,H25b), C26(H26a,H26b), C27(H27a,H27b), C28(H28a,H28b), C29(H29a,
 H29b), C30(H30a,H30b), C31(H31a,H31b), C32(H32a,H32b), C33(H33a,H33b),
 C34(H34a,H34b), C35(H35a,H35b), C36(H36a,H36b), C37(H37a,H37b), C38(H38a,H38b),
  C39(H39a,H39b), C40(H40a,H40b), C41(H41a,H41b), C42(H42a,H42b), C43(H43a,
 H43b), C44(H44a,H44b)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.464
_oxdiff_exptl_absorpt_empirical_full_min 0.622