4-Diazoisochroman-3-imines: A Class of Metal Carbene Precursors for the Synthesis of Isochromene Derivatives.
Ren, Anni; Lang, Bo; Lin, Jialun; Lu, Ping; Wang, Yanguang; The Journal of organic chemistry 82 (2017) 10953–10959; doi:10.1021/acs.joc.7b01860

data_4032956
_publ_section_title
;
 4-Diazoisochroman-3-imines: A Class of Metal Carbene Precursors for the
 Synthesis of Isochromene Derivatives.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10953
_journal_page_last               10959
_journal_paper_doi               10.1021/acs.joc.7b01860
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C25 H21 N O3 S'
_chemical_formula_sum            'C25 H21 N O3 S'
_chemical_formula_weight         415.49
_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
_audit_creation_date             2017-06-29
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Olex2 1.2
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_cell_length_b                   15.8000(10)
_cell_length_c                   16.4284(11)
_cell_measurement_reflns_used    3400
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -32.00   55.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   38.0000  150.0000 87

  2 omega  -88.00   19.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683  -77.0000    0.0000 107

  3 omega  -17.00   85.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7808   77.0000 -120.0000 102
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0125026000
_diffrn_orient_matrix_UB_12      0.0166292000
_diffrn_orient_matrix_UB_13      -0.0372856000
_diffrn_orient_matrix_UB_21      0.0172826000
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_diffrn_orient_matrix_UB_33      0.0115839000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.995
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_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13510
_diffrn_reflns_point_group_measured_fraction_full 0.995
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.187
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_exptl_absorpt_correction_T_min  0.54540
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
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_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
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_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     543
_refine_ls_number_reflns         7374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.1307P)^2^+1.9343P] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_number_total             7374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b01860_si_002.cif
_cod_data_source_block           170628_ran3_186_1_compound_3k
_cod_depositor_comments
'Adding full bibliography for 4032955--4032957.cif.'
_cod_database_code               4032956
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'c h n o S'
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.915
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C32(H32), C33(H33)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C34(H34A,H34B), C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C15(H15), C16(H16), C17(H17), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
  C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C50(H50A,H50B,H50C)
;
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_olex2_submission_special_instructions 'No special instructions were received'