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_7046245
_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         'C48 H80 Ca3 I2 O6 Si2'
_chemical_formula_sum            'C48 H80 Ca3 I2 O6 Si2'
_chemical_formula_weight         1183.34
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-02-09
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3201(2)
_cell_length_b                   17.4852(4)
_cell_length_c                   34.1897(6)
_cell_measurement_reflns_used    42365
_cell_measurement_temperature    180.0(3)
_cell_measurement_theta_max      30.6620
_cell_measurement_theta_min      3.6910
_cell_volume                     7365.1(2)
_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 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_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    -32.00  21.10   0.15    0.46    --   -1.70 -82.00  30.00  354
  2  \w    -33.00  21.00   0.15    0.46    --   -1.70 -82.00 150.00  360
  3  \w    -33.00   0.00   0.15    0.46    --   -1.70 -82.00  60.00  220
  4  \w    -32.00  -5.00   0.15    0.46    --   -1.70 -77.00-120.00  180
  5  \w    -33.00  26.10   0.15    0.46    --   -1.70 -82.00-150.00  394
  6  \w    -52.00 -13.00   0.15    0.46    --   -1.70 -38.00 -90.00  260
  7  \w    -33.00  26.10   0.15    0.46    --   -1.70 -82.00  90.00  394
  8  \w    -32.00  -5.90   0.15    0.46    --    2.00 -82.00-120.00  174
  9  \w    -33.00  33.00   0.15    0.46    --    2.00 -82.00   0.00  440
 10  \w    -33.00  -3.00   0.15    0.46    --    2.00 -82.00 -90.00  200
 11  \w    -16.00   9.05   0.15    0.46    --    2.00 -77.00-180.00  167
 12  \w      8.00  33.05   0.15    0.46    --    2.00 -82.00 -60.00  167
 13  \w     24.00  49.05   0.15    0.46    --    2.00  38.00 150.00  167
 14  \w     25.00  86.05   0.15    0.46    --    2.00  38.00-180.00  407
;
_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      0.0308810000
_diffrn_orient_matrix_UB_12      -0.0018059000
_diffrn_orient_matrix_UB_13      0.0174875000
_diffrn_orient_matrix_UB_21      0.0472666000
_diffrn_orient_matrix_UB_22      -0.0082101000
_diffrn_orient_matrix_UB_23      -0.0110632000
_diffrn_orient_matrix_UB_31      0.0112214000
_diffrn_orient_matrix_UB_32      0.0396930000
_diffrn_orient_matrix_UB_33      -0.0014862000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            141676
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.507
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90775
_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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       block
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.333
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 6064 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.191(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         14478
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0853P)^2^+11.9460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1520
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                13858
_reflns_number_total             14478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01046c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7046245--7046247.cif.'
_cod_database_code               7046245
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C1 H1 Ca1 I1 O1 Si1'
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Rigid bond restraints
 C29, C30, C31, C34, C35, C36, C38, C39, C42, C43, C44, C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C44, O5, O6, C48, C37, C38, C40, C39, C41, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C43, C44, C47, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C31 \\sim C34 \\sim C35 \\sim C36 \\sim C38 \\sim C39 \\sim
C42 \\sim C43 \\sim C44 \\sim C46 \\sim C47 \\sim C48: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\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), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C17(H17), C18(H18), C19(H19), C20(H20)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C)
;
_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 1.200
_oxdiff_exptl_absorpt_empirical_full_min 0.890