Synthesis, Structural Characterization, and Reactivity of a Fluorene-Based Calcium Oxycyclopentadienide Complex
Wei, Baosheng; Li, Heng; Zhang, Wen-Xiong; Xi, Zhenfeng; Organometallics 34 (2015) 1339–; doi:10.1021/acs.organomet.5b00059

data_4087400
_publ_section_title
;
 Synthesis, Structural Characterization, and Reactivity of a
 Fluorene-Based Calcium Oxycyclopentadienide Complex
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1339
_journal_paper_doi               10.1021/acs.organomet.5b00059
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C88 H104 Ca4 O13'
_chemical_formula_sum            'C88 H104 Ca4 O13'
_chemical_formula_weight         1530.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.09 svn.r3130 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                109.69(3)
_cell_angle_beta                 92.03(3)
_cell_angle_gamma                91.21(3)
_cell_formula_units_Z            2
_cell_length_a                   13.492(3)
_cell_length_b                   15.653(3)
_cell_length_c                   19.514(4)
_cell_measurement_reflns_used    12171
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4850
_cell_measurement_theta_min      1.3826
_cell_volume                     3875.4(16)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43331
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.11
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1084
_refine_ls_number_reflns         13643
_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+3.8273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1629
_reflns_number_gt                11735
_reflns_number_total             13643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00059_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        3875.3(13)
_cod_database_code               4087400
_olex2_refinement_description
;
1. Shared sites
{H86A, H86C}
2. Others
 Fixed Uiso: H2(0.044) H3(0.055) H4A(0.06) H5(0.052) H8(0.057) H9(0.065)
 H10(0.059) H1(0.047) H15(0.049) H16(0.061) H17(0.067) H18(0.058) H21(0.067)
 H22(0.075) H23(0.066) H24(0.05) H27A(0.046) H27B(0.046) H28B(0.056)
 H28A(0.056) H29B(0.074) H29A(0.074) H30B(0.062) H30A(0.062) H27C(0.096)
 H27D(0.096) H28D(0.104) H28C(0.104) H29C(0.092) H29D(0.092) H30D(0.082)
 H30C(0.082) H31A(0.078) H31B(0.078) H32B(0.053) H32A(0.053) H33A(0.064)
 H33B(0.064) H34B(0.057) H34A(0.057) H35B(0.056) H35A(0.056) H36B(0.068)
 H36A(0.068) H37B(0.068) H37A(0.068) H38A(0.051) H38B(0.051) H39A(0.056)
 H39B(0.056) H40B(0.061) H40A(0.061) H41B(0.061) H41A(0.061) H42B(0.054)
 H42A(0.054) H43A(0.055) H43B(0.055) H44B(0.076) H44A(0.076) H45A(0.071)
 H45B(0.071) H46B(0.052) H46A(0.052) H48(0.046) H49(0.055) H50(0.061)
 H51(0.057) H54(0.056) H55(0.058) H56(0.055) H57(0.046) H60B(0.076) H60A(0.076)
 H61B(0.08) H61A(0.08) H62A(0.088) H62B(0.088) H63A(0.066) H63B(0.066)
 H60D(0.086) H60C(0.086) H61C(0.091) H61D(0.091) H62C(0.1) H62D(0.1)
 H63C(0.093) H63D(0.093) H64A(0.063) H64B(0.063) H65A(0.06) H65B(0.06)
 H66A(0.062) H66B(0.062) H67B(0.058) H67A(0.058) H69(0.065) H70(0.074)
 H71(0.079) H72(0.072) H75(0.068) H76(0.073) H77(0.068) H4(0.058) H81B(0.148)
 H81A(0.148) H82B(0.132) H82A(0.132) H83B(0.121) H83A(0.121) H84A(0.093)
 H84B(0.093) H85B(0.076) H85A(0.076) H86A(0.076) H86B(0.076) H87A(0.077)
 H87B(0.077) H88A(0.072) H88B(0.072) H85C(0.056) H85D(0.056) H86D(0.073)
 H86C(0.073) H87C(0.09) H87D(0.09) H88C(0.073) H88D(0.073)
 Fixed X: H2(0.0201) H3(-0.1252) H4A(-0.2734) H5(-0.276) H8(-0.235) H9(-0.163)
 H10(0.0046) H1(0.1022) H15(0.232) H16(0.2443) H17(0.3301) H18(0.4021)
 H21(0.4853) H22(0.5338) H23(0.4799) H24(0.377) H27A(-0.0223) H27B(0.0142)
 H28B(-0.0666) H28A(-0.0548) H29B(0.0708) H29A(0.0828) H30B(0.1733)
 H30A(0.2176) H27C(0.0027) H27D(0.0605) H28D(-0.0571) H28C(-0.0546)
 H29C(0.0272) H29D(0.0845) H30D(0.1986) H30C(0.1158) H31A(0.324) H31B(0.2104)
 H32B(0.3239) H32A(0.2073) H33A(0.3673) H33B(0.2737) H34B(0.1721) H34A(0.2747)
 H35B(0.2046) H35A(0.1261) H36B(0.2427) H36A(0.3325) H37B(0.3435) H37A(0.2245)
 H38A(0.2536) H38B(0.3464) H39A(0.045) H39B(0.0088) H40B(-0.1371) H40A(-0.1078)
 H41B(-0.2366) H41A(-0.1849) H42B(-0.1186) H42A(-0.1238) H43A(-0.0904) H43B(-
 0.0823) H44B(-0.1229) H44A(-0.0645) H45A(0.0491) H45B(0.0193) H46B(0.1504)
 H46A(0.1448) H48(0.0325) H49(-0.0908) H50(-0.0653) H51(0.0811) H54(0.2729)
 H55(0.4284) H56(0.4999) H57(0.418) H60B(0.6352) H60A(0.5816) H61B(0.7303)
 H61A(0.6445) H62A(0.5927) H62B(0.6789) H63A(0.4926) H63B(0.5779) H60D(0.5881)
 H60C(0.5443) H61C(0.6562) H61D(0.7249) H62C(0.6994) H62D(0.7072) H63C(0.5367)
 H63D(0.5514) H64A(0.2975) H64B(0.2418) H65A(0.4208) H65B(0.3286) H66A(0.3688)
 H66B(0.4774) H67B(0.4326) H67A(0.5041) H69(0.5611) H70(0.6569) H71(0.5848)
 H72(0.416) H75(0.2146) H76(0.0517) H77(0.0178) H4(0.1457) H81B(0.4828)
 H81A(0.4344) H82B(0.5788) H82A(0.6278) H83B(0.6761) H83A(0.6183) H84A(0.5188)
 H84B(0.5469) H85B(0.224) H85A(0.1119) H86A(0.1567) H86B(0.2693) H87A(0.2179)
 H87B(0.1036) H88A(0.0807) H88B(0.1726) H85C(0.3028) H85D(0.2404) H86D(0.0953)
 H86C(0.1638) H87C(0.1444) H87D(0.053) H88C(0.1349) H88D(0.2228)
 Fixed Y: H2(0.8552) H3(0.9199) H4A(0.895) H5(0.8074) H8(0.6942) H9(0.6018)
 H10(0.5682) H1(0.6217) H15(0.5311) H16(0.5722) H17(0.7075) H18(0.8027)
 H21(0.8837) H22(0.9204) H23(0.8323) H24(0.7048) H27A(0.8607) H27B(0.9555)
 H28B(0.8982) H28A(0.7947) H29B(0.8899) H29A(0.7867) H30B(0.9457) H30A(0.8456)
 H27C(0.8835) H27D(0.9709) H28D(0.9376) H28C(0.8309) H29C(0.8395) H29D(0.9349)
 H30D(0.8376) H30C(0.7588) H31A(0.9933) H31B(1.0167) H32B(1.1296) H32A(1.1201)
 H33A(1.037) H33B(1.0847) H34B(0.9617) H34A(0.9094) H35B(0.7895) H35A(0.7564)
 H36B(0.8236) H36A(0.7991) H37B(0.6884) H37A(0.6765) H38A(0.5601) H38B(0.6138)
 H39A(0.5081) H39B(0.6069) H40B(0.5398) H40A(0.4462) H41B(0.5609) H41A(0.4824)
 H42B(0.6688) H42A(0.6087) H43A(0.4539) H43B(0.4998) H44B(0.3535) H44A(0.3115)
 H45A(0.2932) H45B(0.3849) H46B(0.4451) H46A(0.3684) H48(0.3657) H49(0.2668)
 H50(0.1795) H51(0.194) H54(0.2391) H55(0.302) H56(0.4105) H57(0.4576)
 H60B(0.4022) H60A(0.3881) H61B(0.5062) H61A(0.5225) H62A(0.6412) H62B(0.6252)
 H63A(0.5952) H63B(0.5369) H60D(0.4637) H60C(0.3759) H61C(0.3981) H61D(0.4247)
 H62C(0.5461) H62D(0.5785) H63C(0.5689) H63D(0.6234) H64A(0.2586) H64B(0.3314)
 H65A(0.244) H65B(0.2607) H66A(0.4143) H66B(0.3715) H67B(0.4893) H67A(0.408)
 H69(0.2247) H70(0.121) H71(-0.0087) H72(-0.0395) H75(-0.037) H76(-0.0012)
 H77(0.1347) H4(0.2317) H81B(0.1412) H81A(0.0577) H82B(0.025) H82A(0.0873)
 H83B(0.1864) H83A(0.1287) H84A(0.2486) H84B(0.2766) H85B(0.0793) H85A(0.0601)
 H86A(-0.0857) H86B(-0.0676) H87A(-0.1117) H87B(-0.1152) H88A(0.0295)
 H88B(0.0131) H85C(0.0032) H85D(0.0896) H86D(0.01) H86C(-0.0766) H87C(-0.117)
 H87D(-0.0499) H88C(0.0437) H88D(-0.0271)
 Fixed Z: H2(0.2552) H3(0.2341) H4A(0.2846) H5(0.36) H8(0.442) H9(0.5006)
 H10(0.4881) H1(0.4154) H15(0.452) H16(0.5778) H17(0.6489) H18(0.5962)
 H21(0.4999) H22(0.4006) H23(0.2823) H24(0.2604) H27A(0.4994) H27B(0.5602)
 H28B(0.6362) H28A(0.5839) H29B(0.6992) H29A(0.6469) H30B(0.635) H30A(0.6127)
 H27C(0.4868) H27D(0.5458) H28D(0.6182) H28C(0.5752) H29C(0.6825) H29D(0.6897)
 H30D(0.6223) H30C(0.586) H31A(0.5151) H31B(0.5335) H32B(0.5001) H32A(0.4762)
 H33A(0.3883) H33B(0.3646) H34B(0.3453) H34A(0.3303) H35B(0.2197) H35A(0.1511)
 H36B(0.1032) H36A(0.1494) H37B(0.0373) H37A(0.0245) H38A(0.0676) H38B(0.1196)
 H39A(0.0746) H39B(0.0786) H40B(0.0284) H40A(0.04) H41B(0.1219) H41A(0.1455)
 H42B(0.1853) H42A(0.238) H43A(0.2332) H43B(0.3206) H44B(0.3113) H44A(0.2373)
 H45A(0.3192) H45B(0.382) H46B(0.3453) H46A(0.2659) H48(0.1439) H49(0.0731)
 H50(-0.0486) H51(-0.1022) H54(-0.1348) H55(-0.1355) H56(-0.0303) H57(0.0778)
 H60B(0.2084) H60A(0.2767) H61B(0.298) H61A(0.3559) H62A(0.3252) H62B(0.2675)
 H63A(0.2227) H63B(0.1739) H60D(0.159) H60C(0.1747) H61C(0.2743) H61D(0.2179)
 H62C(0.3455) H62D(0.2756) H63C(0.3509) H63D(0.2952) H64A(0.3181) H64B(0.3828)
 H65A(0.3946) H65B(0.4475) H66A(0.4998) H66B(0.4903) H67B(0.4287) H67A(0.3892)
 H69(0.2155) H70(0.2478) H71(0.2619) H72(0.2401) H75(0.2147) H76(0.1974)
 H77(0.1743) H4(0.1664) H81B(-0.09) H81A(-0.0708) H82B(-0.0298) H82A(-0.0715)
 H83B(0.0351) H83A(0.0766) H84A(0.1075) H84B(0.0382) H85B(-0.1134) H85A(-
 0.0958) H86A(-0.1607) H86B(-0.1263) H87A(-0.0347) H87B(-0.0629) H88A(0.0069)
 H88B(0.0551) H85C(-0.1122) H85D(-0.1122) H86D(-0.1345) H86C(-0.1653) H87C(-
 0.0688) H87D(-0.052) H88C(0.0441) H88D(0.0306)
;
_olex2_submission_special_instructions 'No special instructions were received'