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_7046247
_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         'C60 H72 Ca3 O6'
_chemical_formula_sum            'C60 H72 Ca3 O6'
_chemical_formula_weight         1009.41
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-07
_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                88.6660(10)
_cell_angle_beta                 85.4240(10)
_cell_angle_gamma                80.768(2)
_cell_formula_units_Z            6
_cell_length_a                   10.2714(2)
_cell_length_b                   21.1518(5)
_cell_length_c                   37.3847(5)
_cell_measurement_reflns_used    42053
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      29.8340
_cell_measurement_theta_min      3.7590
_cell_volume                     7990.9(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -37.00  29.00   0.25    2.04    --   -0.10 -77.00-180.00  264
  2  \w     12.00  89.00   0.25    2.04    --   -0.10  57.00 -30.00  308
  3  \w    -12.00  14.00   0.25    2.04    --   -0.10 -77.00 -30.00  104
  4  \w    -77.00 -51.00   0.25    2.04    --   -0.10   0.00  90.00  104
  5  \w    -28.00  13.00   0.25    2.04    --   -0.10   0.00  90.00  164
  6  \w     55.00  89.00   0.25    2.04    --   -0.10   0.00  90.00  136
  7  \w    -51.00 -25.00   0.25    2.04    --   -0.10 -38.00 120.00  104
  8  \w    -48.00 -22.00   0.25    2.04    --   -0.10 -19.00 -90.00  104
  9  \w     -8.00  19.00   0.25    2.04    --   -0.10 -19.00 -90.00  108
 10  \w    -88.00 -63.00   0.25    2.04    --   -0.10 -38.00  30.00  100
 11  \w    -63.00 -38.00   0.25    2.04    --   -0.10 -38.00 150.00  100
 12  \w    -19.00  18.00   0.25    2.04    --   -0.10 -38.00 150.00  148
 13  \w    -89.00 -63.00   0.25    2.04    --   -0.10 -57.00  30.00  104
 14  \w    -38.00 -13.00   0.25    2.04    --   -0.10 -57.00  30.00  100
 15  \w    -19.00   6.00   0.25    2.04    --   -0.10  38.00-180.00  100
 16  \w     -5.00  20.00   0.25    2.04    --   -0.10  38.00-150.00  100
 17  \w    -16.00  46.00   0.25    2.04    --   -0.10  38.00 -60.00  248
 18  \w      3.00  28.00   0.25    2.04    --   -0.10  38.00 -30.00  100
 19  \w    -15.00  11.00   0.25    2.04    --   -0.10 -38.00 -60.00  104
 20  \w    -41.00 -14.00   0.25    2.04    --   -0.10 -38.00  60.00  108
 21  \w    -47.00 -22.00   0.25    2.04    --   -0.10 -19.00-180.00  100
 22  \w    -33.00  -8.00   0.25    2.04    --   -0.10 -82.00 -60.00  100
;
_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      -0.0105570000
_diffrn_orient_matrix_UB_12      0.0024549000
_diffrn_orient_matrix_UB_13      -0.0185349000
_diffrn_orient_matrix_UB_21      -0.0092458000
_diffrn_orient_matrix_UB_22      0.0338820000
_diffrn_orient_matrix_UB_23      0.0010672000
_diffrn_orient_matrix_UB_31      0.0687532000
_diffrn_orient_matrix_UB_32      -0.0005846000
_diffrn_orient_matrix_UB_33      -0.0041998000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            191741
_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         26.022
_diffrn_reflns_theta_min         3.355
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70188
_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    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.816
_refine_diff_density_min         -1.666
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1852
_refine_ls_number_reflns         31373
_refine_ls_number_restraints     761
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0986
_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^)+(0.1083P)^2^+50.4202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2379
_refine_ls_wR_factor_ref         0.2495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25727
_reflns_number_total             31373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01046c2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7046245--7046247.cif.'
_cod_database_code               7046247
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C1 H1 Ca1 Li1 O1'
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     17.19
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C41, C42, C43, C44, C45, C46, C47, C48, C57, C58, C59, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C98, C99, C107, C108, C114, C115
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C165, C166, C167, C168, C169, C170, C171, C172, C173, C174, C175, C176, C177,
 C178, C179, C180
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C121, C122, C123, C124, C125, C126, C127, C128, C129, C130, C131, C132, C145,
 C146, C147, C148, C149, C150, C153, C152, C151, C156
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2, O4, O5, C41, C44, C45, C48, C57, C60, O7, O9, O11, C97, C98, C99, C100,
 C108, C113, C114, C115, C116, O15, O16, O18, C169, C172, C173, C176, C177, C180
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C153, C154, C155, C156
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C57 \\sim C58 \\sim C59 \\sim C60: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C98 \\sim C99 \\sim C107 \\sim C108 \\sim C114 \\sim C115: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C165 \\sim C166 \\sim C167 \\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim
C172 \\sim C173 \\sim C174 \\sim C175 \\sim C176 \\sim C177 \\sim C178 \\sim
C179 \\sim C180: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C127 \\sim
C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132 \\sim C145 \\sim C146 \\sim
C147 \\sim C148 \\sim C149 \\sim C150 \\sim C153 \\sim C152 \\sim C151 \\sim
C156: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C99) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C115)
\\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq: with sigma of 0.001
and sigma for terminal atoms of 0.002
Uanis(C165) \\sim Ueq, Uanis(C166) \\sim Ueq, Uanis(C167) \\sim Ueq,
Uanis(C168) \\sim Ueq, Uanis(C169) \\sim Ueq, Uanis(C170) \\sim Ueq,
Uanis(C171) \\sim Ueq, Uanis(C172) \\sim Ueq, Uanis(C179) \\sim Ueq,
Uanis(C178) \\sim Ueq, Uanis(C180) \\sim Ueq, Uanis(C177) \\sim Ueq,
Uanis(C173) \\sim Ueq, Uanis(C176) \\sim Ueq, Uanis(C175) \\sim Ueq,
Uanis(C174) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C150) \\sim Ueq, Uanis(C149) \\sim Ueq, Uanis(C148) \\sim Ueq,
Uanis(C147) \\sim Ueq, Uanis(C146) \\sim Ueq, Uanis(C145) \\sim Ueq,
Uanis(C151) \\sim Ueq, Uanis(C156) \\sim Ueq, Uanis(C155) \\sim Ueq,
Uanis(C154) \\sim Ueq, Uanis(C153) \\sim Ueq, Uanis(C152) \\sim Ueq,
Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C124) \\sim Ueq,
Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(C121) \\sim Ueq,
Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C129) \\sim Ueq,
Uanis(C130) \\sim Ueq, Uanis(C131) \\sim Ueq, Uanis(C132) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 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), C49(H49A,H49B), C50(H50A,H50B),
  C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
 C60(H60A,H60B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,
 H10B), C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C104(H10I,H10J),
 C105(H10K,H10L), C106(H10M,H10N), C107(H10O,H10P), C108(H10Q,H10R), C109(H10S,
 H10T), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,H11H),
 C114(H11I,H11J), C115(H11K,H11L), C116(H11M,H11N), C117(H11O,H11P), C118(H11Q,
 H11R), C119(H11S,H11T), C120(H12A,H12B), C157(H15A,H15B), C158(H15C,H15D),
 C159(H15E,H15F), C160(H16A,H16B), C161(H16C,H16D), C162(H16E,H16F), C163(H16G,
 H16H), C164(H16I,H16J), C165(H16K,H16L), C166(H16M,H16N), C167(H16O,H16P),
 C168(H16Q,H16R), C169(H16S,H16T), C170(H17A,H17B), C171(H17C,H17D), C172(H17E,
 H17F), C173(H17G,H17H), C174(H17I,H17J), C175(H17K,H17L), C176(H17M,H17N),
 C177(H17O,H17P), C178(H17Q,H17R), C179(H17S,H17T), C180(H18A,H18B)
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),
  C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C35(H35),
 C36(H36), C63(H63), C64(H64), C65(H65), C66(H66), C69(H69), C70(H70), C71(H71),
  C72(H72), C75(H75), C76(H76), C77(H77), C78(H78), C81(H81), C82(H82),
 C83(H83), C84(H84), C87(H87), C88(H88), C89(H89), C90(H90), C93(H93), C94(H94),
  C95(H95), C96(H96), C123(H123), C124(H124), C125(H125), C126(H126),
 C129(H129), C130(H130), C131(H131), C132(H132), C135(H135), C136(H136),
 C137(H137), C138(H138), C141(H141), C142(H142), C143(H143), C144(H144),
 C147(H147), C148(H148), C149(H149), C150(H150), C153(H153), C156(H156),
 C155(H155), C154(H154)
4.c Fitted hexagon refined as free rotating group:
 C153(C152,C151,C156,C155,C154)
;
_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 1.978
_oxdiff_exptl_absorpt_empirical_full_min 0.648