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_4087401
_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         'C25 H21 I O3, C3 H7'
_chemical_formula_sum            'C28 H28 I O3'
_chemical_formula_weight         539.40
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                79.408(3)
_cell_angle_beta                 75.046(4)
_cell_angle_gamma                78.587(4)
_cell_formula_units_Z            2
_cell_length_a                   8.5711(5)
_cell_length_b                   11.9149(4)
_cell_length_c                   12.8621(6)
_cell_measurement_reflns_used    5431
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      28.8820
_cell_measurement_theta_min      3.5180
_cell_volume                     1231.67(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -19.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8579   77.0000 -120.0000 108

  2 omega   -9.00   87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8579   77.0000    0.0000 96

  3 omega  -17.00   10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6392   77.0000  150.0000 27

  4 omega  -40.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6392   77.0000   90.0000 106
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0091441000
_diffrn_orient_matrix_UB_12      -0.0603281000
_diffrn_orient_matrix_UB_13      0.0182561000
_diffrn_orient_matrix_UB_21      0.0309506000
_diffrn_orient_matrix_UB_22      -0.0110615000
_diffrn_orient_matrix_UB_23      -0.0544898000
_diffrn_orient_matrix_UB_31      0.0805241000
_diffrn_orient_matrix_UB_32      0.0006343000
_diffrn_orient_matrix_UB_33      0.0045824000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10061
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                4219
_reflns_number_total             4861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00059_si_002.cif
_cod_data_source_block           exp_4272
_cod_database_code               4087401
_chemical_oxdiff_formula         'C25 H21 I O3'
_reflns_odcompleteness_completeness 99.84
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C21(H21),
 C22(H22), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C26(H26A,H26B,
 H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'